data_nmof04
_audit_creation_date        09-02-25
_audit_creation_method CRYSTALS_ver_12.86

_oxford_structure_analysis_title  'tnmof04 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 .......       0.66
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600        305
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600        178
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....        112
910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          6
915_ALERT_3_G Low Friedel Pair Coverage ......................      66.57 Perc

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

060_ALERT_4_G Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.12

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   0.819(10) ......       3.00 su-Ra
              O6   -H61     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.819(10) ......       3.00 su-Ra
              O7   -H71     1.555   1.555
731_ALERT_1_G Bond    Calc     0.82(3), Rep   0.815(10) ......       3.00 su-Ra
              O7   -H72     1.555   1.555
732_ALERT_1_G Angle   Calc      104(3), Rep   103.8(10) ......       3.00 su-Ra
              H51  -O5   -H52     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      104(3), Rep   104.0(10) ......       3.00 su-Ra
              H61  -O6   -H62     1.555   1.555   1.555
732_ALERT_1_G Angle   Calc      104(3), Rep   104.2(10) ......       3.00 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                    11.2103(4)
_cell_length_b                    9.1455(2)
_cell_length_c                    7.7024(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      789.68(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 =      2.05 Fooo =    504.00 Mu =     24.67 M =    243.84
# Found Formula = C4 H11 N1 Ni1 O7 
# Dc =      2.05 FOOO =    504.00 Mu =     24.67 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         4110
_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     2.051 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              504 
_exptl_absorpt_coefficient_mu     2.467 
 
# Sheldrick geometric approximatio 0.61 0.78 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.69 
_exptl_absorpt_correction_T_max   0.78 
_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             5532 
_reflns_number_total              1551 
_diffrn_reflns_av_R_equivalents   0.041 
# Number of reflections with Friedels Law is 872 
# Number of reflections without Friedels Law is 1551 
# Theoretical number of reflections is about 1200 
 
 
_diffrn_reflns_theta_min          4.457 
_diffrn_reflns_theta_max          30.455 
_diffrn_measured_fraction_theta_max 0.626 
 
_diffrn_reflns_theta_full         25.887 
_diffrn_measured_fraction_theta_full 0.656 
 
 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_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               -14 
_reflns_limit_h_max               14 
_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          -0.78 
_refine_diff_density_max          0.73 
 
 
# 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          1518 
_refine_ls_number_restraints      27 
_refine_ls_number_parameters      137 
_oxford_refine_ls_R_factor_ref    0.0247 
_refine_ls_wR_factor_ref          0.0602 
_refine_ls_goodness_of_fit_ref    0.9165 
_refine_ls_shift/su_max           0.000172 
 
 
# The values computed from all data 
_oxford_reflns_number_all         1518 
_refine_ls_R_factor_all           0.0247 
_refine_ls_wR_factor_all          0.0602 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1283 
_refine_ls_R_factor_gt            0.0207 
_refine_ls_wR_factor_gt           0.0509 
 
_refine_ls_abs_structure_Flack    0.253(15) 
_refine_ls_abs_structure_details  'Flack (1983), 679 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: 
 5.88 8.03 3.82 1.16 
;
# 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 0.09646(3) 0.04542(3) 0.13456(4) 0.0121 1.0000 Uani . . . . . . . 
C1 C 0.2775(2) 0.2541(2) 0.1521(3) 0.0143 1.0000 Uani D . . . . . . 
C2 C 0.2197(2) 0.2724(2) -0.0260(3) 0.0130 1.0000 Uani D . . . . . . 
C3 C 0.1217(2) 0.3880(2) -0.0181(4) 0.0158 1.0000 Uani D . . . . . . 
C4 C 0.0188(2) 0.3604(2) 0.1053(3) 0.0130 1.0000 Uani D . . . . . . 
N1 N 0.1715(2) 0.1312(2) -0.0821(3) 0.0143 1.0000 Uani D . . . . . . 
O1 O 0.24583(18) 0.1453(2) 0.2443(3) 0.0181 1.0000 Uani D . . . . . . 
O2 O 0.3497(2) 0.3490(2) 0.2009(3) 0.0270 1.0000 Uani D . . . . . . 
O3 O 0.00580(19) 0.23982(18) 0.1815(3) 0.0169 1.0000 Uani D . . . . . . 
O4 O -0.05218(17) 0.46678(18) 0.1245(3) 0.0180 1.0000 Uani D . . . . . . 
O5 O 0.17931(19) -0.15640(19) 0.0911(3) 0.0179 1.0000 Uani D . . . . . . 
O6 O -0.06175(18) -0.0332(2) 0.0385(3) 0.0209 1.0000 Uani D . . . . . . 
O7 O 0.0383(2) 0.1989(2) 0.5951(3) 0.0230 1.0000 Uani D . . . . . . 
H11 H 0.2275 0.0754 -0.1200 0.0173 1.0000 Uiso . . . . . . . 
H12 H 0.1188 0.1430 -0.1620 0.0173 1.0000 Uiso . . . . . . . 
H21 H 0.2807 0.3038 -0.1091 0.0157 1.0000 Uiso . . . . . . . 
H31 H 0.1589 0.4794 0.0153 0.0189 1.0000 Uiso . . . . . . . 
H32 H 0.0887 0.3972 -0.1341 0.0189 1.0000 Uiso . . . . . . . 
H51 H 0.198(3) -0.175(4) -0.009(2) 0.0211 1.0000 Uiso D . . . . . . 
H52 H 0.121(2) -0.207(3) 0.108(4) 0.0211 1.0000 Uiso D . . . . . . 
H61 H -0.091(4) 0.017(3) -0.039(4) 0.0250 1.0000 Uiso D . . . . . . 
H62 H -0.066(4) -0.1167(16) 0.000(4) 0.0250 1.0000 Uiso D . . . . . . 
H71 H -0.024(2) 0.186(4) 0.649(5) 0.0276 1.0000 Uiso D . . . . . . 
H72 H 0.041(3) 0.130(3) 0.528(4) 0.0276 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 0.01380(17) 0.01003(12) 0.01242(19) 0.00049(10) 0.00044(9) -0.00059(10) 
C1 0.0149(14) 0.0135(8) 0.0146(16) 0.0025(9) 0.0005(7) -0.0013(7) 
C2 0.0143(15) 0.0131(9) 0.0115(16) 0.0009(8) 0.0007(7) -0.0005(8) 
C3 0.0168(15) 0.0131(9) 0.0176(18) 0.0064(9) 0.0036(7) 0.0023(8) 
C4 0.0144(13) 0.0115(8) 0.0130(16) -0.0025(8) -0.0012(6) 0.0000(7) 
N1 0.0167(13) 0.0137(7) 0.0127(13) -0.0027(7) 0.0009(6) 0.0021(7) 
O1 0.0216(12) 0.0162(7) 0.0166(13) 0.0052(7) -0.0047(6) -0.0049(6) 
O2 0.0308(14) 0.0253(9) 0.0249(15) 0.0031(8) -0.0082(8) -0.0144(8) 
O3 0.0211(12) 0.0106(7) 0.0190(12) 0.0010(6) 0.0048(6) 0.0021(6) 
O4 0.0241(11) 0.0136(6) 0.0162(12) -0.0001(8) 0.0048(6) 0.0072(6) 
O5 0.0198(13) 0.0166(7) 0.0173(14) -0.0030(7) -0.0007(6) 0.0020(7) 
O6 0.0200(12) 0.0134(7) 0.0293(14) 0.0014(8) -0.0082(6) 0.0007(6) 
O7 0.0270(14) 0.0173(8) 0.0247(17) -0.0010(7) 0.0007(7) -0.0004(7) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.4956(10) 
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 2.051(2)    yes
Ni1 . N1 . 2.027(2)    yes
Ni1 . O1 . 2.0864(19)    yes
Ni1 . O3 . 2.0796(17)    yes
Ni1 . O5 . 2.0932(18)    yes
Ni1 . O6 . 2.0519(19)    yes
C1 . C2 . 1.526(3)    yes
C1 . O1 . 1.273(3)    yes
C1 . O2 . 1.245(3)    yes
C2 . C3 . 1.526(3)    yes
C2 . N1 . 1.465(3)    yes
C2 . H21 . 0.980    no
C3 . C4 . 1.516(3)    yes
C3 . H31 . 0.968    no
C3 . H32 . 0.971    no
C4 . O3 . 1.257(3)    yes
C4 . O4 . 1.265(3)    yes
N1 . H11 . 0.861    no
N1 . H12 . 0.860    no
O5 . H51 . 0.818(10)    no
O5 . H52 . 0.818(10)    no
O6 . H61 . 0.819(10)    no
O6 . H62 . 0.819(10)    no
O7 . H71 . 0.819(10)    no
O7 . H72 . 0.815(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 . N1 . 168.83(8)    yes
O4 3_545 Ni1 . O1 . 88.92(8)    yes
N1 . Ni1 . O1 . 80.27(9)    yes
O4 3_545 Ni1 . O3 . 91.39(7)    yes
N1 . Ni1 . O3 . 90.85(8)    yes
O1 . Ni1 . O3 . 86.99(8)    yes
O4 3_545 Ni1 . O5 . 86.73(8)    yes
N1 . Ni1 . O5 . 91.47(8)    yes
O1 . Ni1 . O5 . 95.44(8)    yes
O3 . Ni1 . O5 . 176.89(8)    yes
O4 3_545 Ni1 . O6 . 89.67(9)    yes
N1 . Ni1 . O6 . 101.38(9)    yes
O1 . Ni1 . O6 . 173.35(8)    yes
O3 . Ni1 . O6 . 86.55(8)    yes
O5 . Ni1 . O6 . 90.97(8)    yes
C2 . C1 . O1 . 118.0(2)    yes
C2 . C1 . O2 . 118.1(2)    yes
O1 . C1 . O2 . 123.9(2)    yes
C1 . C2 . C3 . 110.2(2)    yes
C1 . C2 . N1 . 108.96(18)    yes
C3 . C2 . N1 . 110.9(2)    yes
C1 . C2 . H21 . 108.8    no
C3 . C2 . H21 . 109.0    no
N1 . C2 . H21 . 108.9    no
C2 . C3 . C4 . 117.21(18)    yes
C2 . C3 . H31 . 107.4    no
C4 . C3 . H31 . 107.8    no
C2 . C3 . H32 . 107.3    no
C4 . C3 . H32 . 107.5    no
H31 . C3 . H32 . 109.5    no
C3 . C4 . O3 . 121.8(2)    yes
C3 . C4 . O4 . 115.05(19)    yes
O3 . C4 . O4 . 123.2(2)    yes
C2 . N1 . Ni1 . 104.57(15)    yes
C2 . N1 . H11 . 110.7    no
Ni1 . N1 . H11 . 110.7    no
C2 . N1 . H12 . 110.7    no
Ni1 . N1 . H12 . 110.7    no
H11 . N1 . H12 . 109.4    no
C1 . O1 . Ni1 . 109.87(16)    yes
Ni1 . O3 . C4 . 127.74(16)    yes
C4 . O4 . Ni1 3_555 121.84(18)    yes
Ni1 . O5 . H51 . 117(3)    no
Ni1 . O5 . H52 . 97(2)    no
H51 . O5 . H52 . 103.8(10)    no
Ni1 . O6 . H61 . 114(3)    no
Ni1 . O6 . H62 . 120(3)    no
H61 . O6 . H62 . 104.0(10)    no
H71 . O7 . H72 . 104.2(10)    no
