data_nmof03
_audit_creation_date        09-02-25
_audit_creation_method CRYSTALS_ver_12.86

_oxford_structure_analysis_title  'tnmof03 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        268
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600        208
910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          7
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....         64
915_ALERT_3_G Low Friedel Pair Coverage ......................      69.68 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       H62    ..  H72     ..       2.08 Ang.

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

060_ALERT_4_G Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.11

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc.  Here, residual absorption errors from the pressure
cell are an obvious source of further systematic error.

731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.818(10) ......       3.00 su-Ra
              O5   -H51     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(4), Rep   0.820(10) ......       4.00 su-Ra
              O5   -H52     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(4), Rep   0.819(10) ......       4.00 su-Ra
              O6   -H61     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.822(10) ......       3.00 su-Ra
              O7   -H71     1.555   1.555
732_ALERT_1_G Angle   Calc      104(4), Rep   104.4(10) ......       4.00 su-Ra
              H51  -O5   -H52     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      104(4), Rep   104.0(10) ......       4.00 su-Ra
              H61  -O6   -H62     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      104(4), Rep   104.1(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.

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                    12.1614(4)
_cell_length_b                    8.9501(2)
_cell_length_c                    7.5626(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      823.16(5)
 
_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 =      1.97 Fooo =    504.00 Mu =     23.66 M =    243.84
# Found Formula = C4 H11 N1 Ni1 O7 
# Dc =      1.97 FOOO =    504.00 Mu =     23.66 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         3691
_cell_measurement_theta_min              4
_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     1.967 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              504 
_exptl_absorpt_coefficient_mu     2.366 
 
# Sheldrick geometric approximatio 0.62 0.79 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.70 
_exptl_absorpt_correction_T_max   0.79 
_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             6193 
_reflns_number_total              1685 
_diffrn_reflns_av_R_equivalents   0.049 
# Number of reflections with Friedels Law is 946 
# Number of reflections without Friedels Law is 1685 
# Theoretical number of reflections is about 1253 
 
 
_diffrn_reflns_theta_min          3.905 
_diffrn_reflns_theta_max          30.477 
_diffrn_measured_fraction_theta_max 0.648 
 
_diffrn_reflns_theta_full         25.600 
_diffrn_measured_fraction_theta_full 0.691 
 
 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        8 
_reflns_limit_h_min               -16 
_reflns_limit_h_max               16 
_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          -0.98 
_refine_diff_density_max          0.88 
 
 
# 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          1672 
_refine_ls_number_restraints      27 
_refine_ls_number_parameters      137 
_oxford_refine_ls_R_factor_ref    0.0348 
_refine_ls_wR_factor_ref          0.0608 
_refine_ls_goodness_of_fit_ref    0.9539 
_refine_ls_shift/su_max           0.000069 
 
 
# The values computed from all data 
_oxford_reflns_number_all         1672 
_refine_ls_R_factor_all           0.0348 
_refine_ls_wR_factor_all          0.0608 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1362 
_refine_ls_R_factor_gt            0.0282 
_refine_ls_wR_factor_gt           0.0536 
 
_refine_ls_abs_structure_Flack    0.27(2) 
_refine_ls_abs_structure_details  'Flack (1983), 739 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: 
 4.12 4.39 0.937 
;
# 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 0.07982(4) 0.06499(4) 0.12374(7) 0.0166 1.0000 Uani . . . . . . . 
C1 C 0.2733(3) 0.2247(3) 0.2056(5) 0.0190 1.0000 Uani D . . . . . . 
C2 C 0.2441(3) 0.2655(3) 0.0170(5) 0.0181 1.0000 Uani D . . . . . . 
C3 C 0.1724(3) 0.4072(3) 0.0136(6) 0.0204 1.0000 Uani D . . . . . . 
C4 C 0.0651(3) 0.4006(3) 0.1174(6) 0.0168 1.0000 Uani D . . . . . . 
O1 O 0.2104(2) 0.1312(3) 0.2833(4) 0.0213 1.0000 Uani D . . . . . . 
O2 O 0.3525(2) 0.2880(3) 0.2798(4) 0.0266 1.0000 Uani D . . . . . . 
O3 O 0.0178(2) 0.2776(2) 0.1463(5) 0.0229 1.0000 Uani D . . . . . . 
O4 O 0.0245(3) 0.5241(2) 0.1650(5) 0.0285 1.0000 Uani D . . . . . . 
O5 O 0.1383(2) -0.1532(2) 0.1159(5) 0.0203 1.0000 Uani D . . . . . . 
O6 O -0.0409(3) 0.0109(3) -0.0553(6) 0.0413 1.0000 Uani D . . . . . . 
O7 O 0.0936(3) 0.2182(3) 0.5868(5) 0.0308 1.0000 Uani D . . . . . . 
N1 N 0.1854(3) 0.1396(3) -0.0650(5) 0.0174 1.0000 Uani D . . . . . . 
H11 H 0.2308 0.0702 -0.0945 0.0209 1.0000 Uiso . . . . . . . 
H12 H 0.1499 0.1689 -0.1569 0.0209 1.0000 Uiso . . . . . . . 
H21 H 0.3120 0.2844 -0.0492 0.0217 1.0000 Uiso . . . . . . . 
H31 H 0.2159 0.4886 0.0614 0.0245 1.0000 Uiso . . . . . . . 
H32 H 0.1544 0.4282 -0.1088 0.0245 1.0000 Uiso . . . . . . . 
H51 H 0.144(3) -0.201(4) 0.024(3) 0.0244 1.0000 Uiso D . . . . . . 
H52 H 0.091(3) -0.198(4) 0.172(5) 0.0244 1.0000 Uiso D . . . . . . 
H61 H -0.075(4) 0.057(4) -0.131(6) 0.0495 1.0000 Uiso D . . . . . . 
H62 H -0.064(4) -0.075(2) -0.065(7) 0.0495 1.0000 Uiso D . . . . . . 
H71 H 0.127(3) 0.195(6) 0.497(4) 0.0369 1.0000 Uiso D . . . . . . 
H72 H 0.0296(14) 0.197(5) 0.564(6) 0.0369 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 0.0173(2) 0.01234(14) 0.0200(3) -0.00090(19) 0.00087(18) 0.00013(16) 
C1 0.017(2) 0.0147(13) 0.025(3) -0.0003(14) -0.0001(12) 0.0046(12) 
C2 0.0160(19) 0.0151(14) 0.023(3) 0.0006(13) 0.0015(12) 0.0008(12) 
C3 0.018(2) 0.0153(16) 0.027(3) 0.0042(13) 0.0051(13) 0.0036(11) 
C4 0.0230(19) 0.0124(11) 0.015(2) 0.0019(13) 0.0022(14) 0.0040(10) 
O1 0.0281(18) 0.0202(12) 0.016(2) 0.0044(11) -0.0041(10) -0.0026(10) 
O2 0.0294(18) 0.0285(13) 0.022(2) 0.0005(12) -0.0089(11) -0.0085(11) 
O3 0.0230(15) 0.0131(9) 0.033(2) -0.0016(12) 0.0083(11) 0.0014(9) 
O4 0.0355(18) 0.0123(11) 0.038(3) 0.0029(11) 0.0169(12) 0.0064(9) 
O5 0.0228(15) 0.0151(10) 0.0231(19) -0.0020(12) 0.0014(11) -0.0002(8) 
O6 0.040(2) 0.0211(13) 0.063(3) 0.0020(14) -0.0291(15) -0.0018(12) 
O7 0.0348(19) 0.0321(13) 0.025(3) 0.0009(12) -0.0024(11) 0.0013(13) 
N1 0.022(2) 0.0162(13) 0.014(2) -0.0030(11) 0.0008(10) 0.0002(11) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.4171(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 2.073(3)    yes
Ni1 . O1 . 2.081(3)    yes
Ni1 . O3 . 2.054(2)    yes
Ni1 . O5 . 2.079(2)    yes
Ni1 . O6 . 2.055(3)    yes
Ni1 . N1 . 2.033(3)    yes
C1 . C2 . 1.514(5)    yes
C1 . O1 . 1.277(4)    yes
C1 . O2 . 1.250(4)    yes
C2 . C3 . 1.539(4)    yes
C2 . N1 . 1.471(4)    yes
C2 . H21 . 0.980    no
C3 . C4 . 1.525(4)    yes
C3 . H31 . 0.970    no
C3 . H32 . 0.970    no
C4 . O3 . 1.261(3)    yes
C4 . O4 . 1.263(3)    yes
O5 . H51 . 0.818(10)    no
O5 . H52 . 0.820(10)    no
O6 . H61 . 0.819(10)    no
O6 . H62 . 0.821(10)    no
O7 . H71 . 0.822(10)    no
O7 . H72 . 0.818(10)    no
N1 . H11 . 0.860    no
N1 . H12 . 0.860    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 . O1 . 94.02(13)    yes
O4 3_545 Ni1 . O3 . 82.81(11)    yes
O1 . Ni1 . O3 . 88.17(11)    yes
O4 3_545 Ni1 . O5 . 93.75(11)    yes
O1 . Ni1 . O5 . 91.32(11)    yes
O3 . Ni1 . O5 . 176.48(14)    yes
O4 3_545 Ni1 . O6 . 91.67(17)    yes
O1 . Ni1 . O6 . 173.98(16)    yes
O3 . Ni1 . O6 . 90.61(13)    yes
O5 . Ni1 . O6 . 90.25(12)    yes
O4 3_545 Ni1 . N1 . 170.36(11)    yes
O1 . Ni1 . N1 . 80.31(13)    yes
O3 . Ni1 . N1 . 89.19(12)    yes
O5 . Ni1 . N1 . 94.16(12)    yes
O6 . Ni1 . N1 . 93.79(16)    yes
C2 . C1 . O1 . 116.9(3)    yes
C2 . C1 . O2 . 119.6(3)    yes
O1 . C1 . O2 . 123.5(3)    yes
C1 . C2 . C3 . 110.3(3)    yes
C1 . C2 . N1 . 109.0(3)    yes
C3 . C2 . N1 . 110.4(3)    yes
C1 . C2 . H21 . 109.0    no
C3 . C2 . H21 . 109.0    no
N1 . C2 . H21 . 109.0    no
C2 . C3 . C4 . 116.4(3)    yes
C2 . C3 . H31 . 107.7    no
C4 . C3 . H31 . 107.7    no
C2 . C3 . H32 . 107.7    no
C4 . C3 . H32 . 107.7    no
H31 . C3 . H32 . 109.5    no
C3 . C4 . O3 . 120.9(2)    yes
C3 . C4 . O4 . 116.6(2)    yes
O3 . C4 . O4 . 122.4(3)    yes
C1 . O1 . Ni1 . 112.1(2)    yes
C4 . O3 . Ni1 . 128.8(2)    yes
C4 . O4 . Ni1 3_555 127.9(2)    yes
Ni1 . O5 . H51 . 123(3)    no
Ni1 . O5 . H52 . 102(3)    no
H51 . O5 . H52 . 104.4(10)    no
Ni1 . O6 . H61 . 135(3)    no
Ni1 . O6 . H62 . 121(3)    no
H61 . O6 . H62 . 104.0(10)    no
H71 . O7 . H72 . 104.1(10)    no
C2 . N1 . Ni1 . 105.2(2)    yes
C2 . N1 . H11 . 110.5    no
Ni1 . N1 . H11 . 110.5    no
C2 . N1 . H12 . 110.6    no
Ni1 . N1 . H12 . 110.5    no
H11 . N1 . H12 . 109.5    no
