data_nmof09
_audit_creation_date        09-02-25
_audit_creation_method CRYSTALS_ver_12.86

_oxford_structure_analysis_title  'tnmof09 in P2(1)2(1)2(1)'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
_publ_contact_author_name         'Jamie A. Gould' 
_publ_contact_author_address 
; 
 Department of Chemistry, 
 University of Liverpool, 
 Crown Street, 
 Liverpool, 
 L69 7ZD 
; 
 
_publ_contact_author_email        'j.a.gould@liv.ac.uk' 
 
_publ_section_exptl_refinement 
; 
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.69
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600        233
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600        161
910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          5
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....         70
915_ALERT_3_G Low Friedel Pair Coverage ......................      69.60 Perc

All of the above alerts are caused by shading of the high-pressure cell.

417_ALERT_2_C Short Inter D-H..H-D       H12    ..  H71     ..       2.04 Ang.

Short contacts are expected at high-pressure (see full text).

779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF ......      44.35 Deg.
              NI1  -C2   -N1      1.555   1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.822(10) ......       3.00 su-Ra
              O5   -H52     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(4), Rep   0.816(10) ......       4.00 su-Ra
              O7   -H71     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.816(10) ......       3.00 su-Ra
              O7   -H72     1.555   1.555
732_ALERT_1_G Angle   Calc      104(4), Rep   103.7(10) ......       4.00 su-Ra
              H51  -O5   -H52     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      105(3), Rep   104.0(10) ......       3.00 su-Ra
              H61  -O6   -H62     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      105(4), Rep   104.6(10) ......       4.00 su-Ra
              H71  -O7   -H72     1.555   1.555   1.555

The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.

764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.14 Ratio

No action taken.

199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
791_ALERT_4_G The Model has Chirality at C2      (Verify) ....          S

This is correct.

860_ALERT_3_G Note: Number of Least-Squares Restraints .......         27

1,2 and 1,3 restraints were applied to the aspartate ligand.  
See text for full details.
; 
 
_publ_section_exptl_prep 
; 
? 
; 
 
 
#end of refcif 
_cell_length_a                    10.5597(8)
_cell_length_b                    8.9766(5)
_cell_length_c                    7.5071(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      711.60(9)
 
_symmetry_cell_setting            'Orthorhombic' 
_symmetry_space_group_name_H-M    'P 21 21 21 ' 
_symmetry_space_group_name_Hall   'P 2ac 2ab ' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 'x+1/2,-y+1/2,-z'
 '-x,y+1/2,-z+1/2'
 '-x+1/2,-y,z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Ni      0.3393   1.1124  12.8376   3.8785   7.2920   0.2565   4.4438  12.1763
   2.3800  66.3421   1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    4

# Given Formula = C4 H11 N1 Ni1 O7 
# Dc =      2.28 Fooo =    504.00 Mu =     27.37 M =    243.84
# Found Formula = C4 H11 N1 Ni1 O7 
# Dc =      2.28 FOOO =    504.00 Mu =     27.37 M =    243.84

_chemical_formula_sum             'C4 H11 N1 Ni1 O7'
_chemical_formula_moiety          'C4 H9 N Ni O6, H2 O'
_chemical_compound_source                ?
_chemical_formula_weight            243.84
 
 
_cell_measurement_reflns_used         3629
_cell_measurement_theta_min              2
_cell_measurement_theta_max             20
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.10 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_max           0.20 
 
_exptl_crystal_density_diffrn     2.276 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              504 
_exptl_absorpt_coefficient_mu     2.737 
 
# Sheldrick geometric approximatio 0.58 0.76 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.64 
_exptl_absorpt_correction_T_max   0.76 
_diffrn_measurement_device        'Bruker Kappa Apex2' 
_diffrn_measurement_device_type   'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_wavelength           0.4769
_diffrn_source                   synchrotron
_diffrn_measurement_method        ω 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Apex2 (Bruker AXS, 2006)' 
_computing_cell_refinement        'Apex2 (Bruker AXS, 2006)' 
_computing_data_reduction         'Apex2 (Bruker AXS, 2006)' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number             5346 
_reflns_number_total              1474 
_diffrn_reflns_av_R_equivalents   0.029 
# Number of reflections with Friedels Law is 836 
# Number of reflections without Friedels Law is 1474 
# Theoretical number of reflections is about 1089 
 
 
_diffrn_reflns_theta_min          3.538 
_diffrn_reflns_theta_max          30.542 
_diffrn_measured_fraction_theta_max 0.656 
 
_diffrn_reflns_theta_full         25.044 
_diffrn_measured_fraction_theta_full 0.694 
 
 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_reflns_limit_h_min               -13 
_reflns_limit_h_max               13 
_reflns_limit_k_min               0 
_reflns_limit_k_max               12 
_reflns_limit_l_min               0 
_reflns_limit_l_max               9 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    geom
 
_refine_diff_density_min          -1.21 
_refine_diff_density_max          1.22 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          1460 
_refine_ls_number_restraints      27 
_refine_ls_number_parameters      137 
_oxford_refine_ls_R_factor_ref    0.0277 
_refine_ls_wR_factor_ref          0.0598 
_refine_ls_goodness_of_fit_ref    0.9294 
_refine_ls_shift/su_max           0.000443 
 
 
# The values computed from all data 
_oxford_reflns_number_all         1460 
_refine_ls_R_factor_all           0.0277 
_refine_ls_wR_factor_all          0.0598 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1201 
_refine_ls_R_factor_gt            0.0220 
_refine_ls_wR_factor_gt           0.0496 
 
_refine_ls_abs_structure_Flack    0.279(19) 
_refine_ls_abs_structure_details  'Flack (1983), 638 Friedel-pairs' 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  'ad' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     mixed          # none, undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.48 5.61 2.30 0.494 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Flack, H. D. (1983). Acta Cryst. A39, 876-881. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
 
Bruker Analytical X-ray Systems, Inc., 2006. Apex2, 
Version 2 User Manual, M86-E01078, Madison, WI. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Ni1 Ni 0.09733(3) 0.03849(4) 0.12657(6) 0.0130 1.0000 Uani . . . . . . . 
C1 C 0.2798(3) 0.2571(3) 0.1364(5) 0.0141 1.0000 Uani D . . . . . . 
C2 C 0.2180(3) 0.2721(3) -0.0449(4) 0.0136 1.0000 Uani D . . . . . . 
C3 C 0.1141(3) 0.3875(3) -0.0360(4) 0.0145 1.0000 Uani D . . . . . . 
C4 C 0.0115(3) 0.3565(3) 0.0988(4) 0.0127 1.0000 Uani D . . . . . . 
N1 N 0.1674(2) 0.1275(2) -0.0979(4) 0.0140 1.0000 Uani D . . . . . . 
O1 O 0.2587(2) 0.1409(2) 0.2258(4) 0.0184 1.0000 Uani D . . . . . . 
O2 O 0.3473(3) 0.3620(3) 0.1919(4) 0.0242 1.0000 Uani D . . . . . . 
O3 O 0.0038(2) 0.2357(2) 0.1814(3) 0.0153 1.0000 Uani D . . . . . . 
O4 O -0.06633(17) 0.4627(2) 0.1225(4) 0.0161 1.0000 Uani D . . . . . . 
O5 O 0.1859(2) -0.1641(2) 0.0770(3) 0.0168 1.0000 Uani D . . . . . . 
O6 O -0.0755(2) -0.0446(2) 0.0563(3) 0.0185 1.0000 Uani D . . . . . . 
O7 O 0.0310(3) 0.1945(3) 0.5842(4) 0.0215 1.0000 Uani D . . . . . . 
H11 H 0.2264 0.0721 -0.1407 0.0167 1.0000 Uiso . . . . . . . 
H12 H 0.1086 0.1383 -0.1760 0.0167 1.0000 Uiso . . . . . . . 
H21 H 0.2817 0.3039 -0.1319 0.0164 1.0000 Uiso . . . . . . . 
H31 H 0.1524 0.4825 -0.0067 0.0174 1.0000 Uiso . . . . . . . 
H32 H 0.0749 0.3936 -0.1526 0.0174 1.0000 Uiso . . . . . . . 
H51 H 0.207(4) -0.177(4) -0.027(2) 0.0202 1.0000 Uiso D . . . . . . 
H52 H 0.134(3) -0.231(3) 0.095(5) 0.0202 1.0000 Uiso D . . . . . . 
H61 H -0.081(4) 0.001(3) -0.038(2) 0.0222 1.0000 Uiso D . . . . . . 
H62 H -0.066(4) -0.1313(16) 0.027(4) 0.0222 1.0000 Uiso D . . . . . . 
H71 H -0.032(3) 0.181(4) 0.645(6) 0.0258 1.0000 Uiso D . . . . . . 
H72 H 0.038(4) 0.118(3) 0.525(5) 0.0258 1.0000 Uiso D . . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01233(19) 0.01080(13) 0.0159(2) 0.00049(15) 0.00048(13) -0.00093(13) 
C1 0.0123(16) 0.0134(10) 0.0166(19) 0.0006(12) -0.0003(10) -0.0004(9) 
C2 0.0116(18) 0.0143(11) 0.015(2) -0.0005(10) 0.0015(9) -0.0011(10) 
C3 0.017(2) 0.0144(11) 0.012(2) 0.0042(10) 0.0023(9) 0.0018(11) 
C4 0.0102(16) 0.0127(10) 0.015(2) -0.0003(10) -0.0015(8) 0.0011(9) 
N1 0.0164(16) 0.0127(9) 0.0127(18) -0.0016(9) -0.0004(8) 0.0013(8) 
O1 0.0210(15) 0.0157(9) 0.0184(17) 0.0039(8) -0.0061(8) -0.0037(8) 
O2 0.0304(18) 0.0212(10) 0.0211(18) 0.0026(9) -0.0052(9) -0.0132(10) 
O3 0.0171(15) 0.0108(8) 0.0179(16) 0.0015(7) 0.0035(7) 0.0004(8) 
O4 0.0151(12) 0.0132(7) 0.0199(15) -0.0005(12) 0.0030(7) 0.0043(7) 
O5 0.0149(15) 0.0164(9) 0.0192(17) -0.0019(8) 0.0008(7) 0.0008(8) 
O6 0.0167(14) 0.0135(8) 0.0254(16) 0.0012(9) -0.0044(7) 0.0007(9) 
O7 0.0223(17) 0.0163(9) 0.026(2) -0.0018(9) 0.0009(8) 0.0009(8) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.3806(5) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Ni1 . O4 3_545 2.029(3)    yes
Ni1 . C1 . 2.751(3)    yes
Ni1 . C2 . 2.771(3)    yes
Ni1 . N1 . 2.006(3)    yes
Ni1 . O1 . 2.075(2)    yes
Ni1 . O3 . 2.069(2)    yes
Ni1 . O5 . 2.079(2)    yes
Ni1 . O6 . 2.041(2)    yes
C1 . C2 . 1.515(4)    yes
C1 . O1 . 1.260(3)    yes
C1 . O2 . 1.252(3)    yes
C2 . C3 . 1.510(4)    yes
C2 . N1 . 1.459(3)    yes
C2 . H21 . 0.980    no
C3 . C4 . 1.508(4)    yes
C3 . H31 . 0.970    no
C3 . H32 . 0.970    no
C4 . O3 . 1.252(3)    yes
C4 . O4 . 1.271(3)    yes
N1 . H11 . 0.860    no
N1 . H12 . 0.860    no
O5 . H51 . 0.820(10)    no
O5 . H52 . 0.822(10)    no
O6 . H61 . 0.820(10)    no
O6 . H62 . 0.815(10)    no
O7 . H71 . 0.816(10)    no
O7 . H72 . 0.816(10)    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O4 3_545 Ni1 . C1 . 109.11(9)    yes
O4 3_545 Ni1 . C2 . 139.38(9)    yes
C1 . Ni1 . C2 . 31.84(9)    yes
O4 3_545 Ni1 . N1 . 166.55(9)    yes
C1 . Ni1 . N1 . 58.67(10)    yes
C2 . Ni1 . N1 . 30.55(9)    yes
O4 3_545 Ni1 . O1 . 87.00(9)    yes
C1 . Ni1 . O1 . 25.72(8)    yes
C2 . Ni1 . O1 . 56.89(9)    yes
N1 . Ni1 . O1 . 79.76(11)    yes
O4 3_545 Ni1 . O3 . 91.45(9)    yes
C1 . Ni1 . O3 . 73.67(9)    yes
C2 . Ni1 . O3 . 70.39(9)    yes
N1 . Ni1 . O3 . 90.13(9)    yes
O1 . Ni1 . O3 . 86.65(10)    yes
O4 3_545 Ni1 . O5 . 86.87(9)    yes
C1 . Ni1 . O5 . 108.28(9)    yes
C2 . Ni1 . O5 . 111.84(9)    yes
N1 . Ni1 . O5 . 91.84(10)    yes
O1 . Ni1 . O5 . 94.73(9)    yes
O4 3_545 Ni1 . O6 . 88.45(9)    yes
C1 . Ni1 . O6 . 153.37(9)    yes
C2 . Ni1 . O6 . 124.60(9)    yes
N1 . Ni1 . O6 . 104.97(11)    yes
O1 . Ni1 . O6 . 171.60(10)    yes
O3 . Ni1 . O5 . 177.76(10)    yes
O3 . Ni1 . O6 . 86.40(10)    yes
O5 . Ni1 . O6 . 92.07(10)    yes
Ni1 . C1 . C2 . 74.81(15)    yes
Ni1 . C1 . O1 . 45.59(14)    yes
C2 . C1 . O1 . 118.4(2)    yes
Ni1 . C1 . O2 . 160.7(3)    yes
C2 . C1 . O2 . 118.5(2)    yes
O1 . C1 . O2 . 123.1(3)    yes
C1 . C2 . Ni1 . 73.35(15)    yes
C1 . C2 . C3 . 109.5(2)    yes
Ni1 . C2 . C3 . 99.44(17)    yes
C1 . C2 . N1 . 108.9(2)    yes
Ni1 . C2 . N1 . 44.35(14)    yes
C3 . C2 . N1 . 110.8(2)    yes
C1 . C2 . H21 . 109.2    no
Ni1 . C2 . H21 . 147.7    no
C3 . C2 . H21 . 109.2    no
N1 . C2 . H21 . 109.2    no
C2 . C3 . C4 . 115.2(2)    yes
C2 . C3 . H31 . 108.0    no
C4 . C3 . H31 . 108.0    no
C2 . C3 . H32 . 108.0    no
C4 . C3 . H32 . 108.0    no
H31 . C3 . H32 . 109.5    no
C3 . C4 . O3 . 122.6(2)    yes
C3 . C4 . O4 . 114.9(2)    yes
O3 . C4 . O4 . 122.5(3)    yes
C2 . N1 . Ni1 . 105.10(19)    yes
C2 . N1 . H11 . 110.6    no
Ni1 . N1 . H11 . 110.6    no
C2 . N1 . H12 . 110.6    no
Ni1 . N1 . H12 . 110.6    no
H11 . N1 . H12 . 109.5    no
C1 . O1 . Ni1 . 108.70(19)    yes
C4 . O3 . Ni1 . 127.7(2)    yes
C4 . O4 . Ni1 3_555 119.1(2)    yes
Ni1 . O5 . H51 . 115(3)    no
Ni1 . O5 . H52 . 108(3)    no
H51 . O5 . H52 . 103.7(10)    no
Ni1 . O6 . H61 . 96(3)    no
Ni1 . O6 . H62 . 108(3)    no
H61 . O6 . H62 . 104.0(10)    no
H71 . O7 . H72 . 104.6(10)    no
