data_nmof01
_audit_creation_date        09-02-27
_audit_creation_method CRYSTALS_ver_12.86

_oxford_structure_analysis_title  'tnmof01 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 
; 
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF ......      43.27 Deg.
              NI1  -C1   -O1      1.555   1.555   1.555
779_ALERT_4_B Suspect or Irrelevant (Bond) Angle in CIF ......      44.47 Deg.
              NI1  -C2   -N1      1.555   1.555   1.555
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.14 Ratio
153_ALERT_1_G The su's on the Cell Axes   are Equal (x 100000)         20 Ang.

No action taken.


232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni1    --  O5      ..      14.23 su
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  O1      ..       5.21 su
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  N1      ..       6.45 su

Ton Spek has observed that these errors usually occur for 'good' data sets.

912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         82
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          5
915_ALERT_3_G Low Friedel Pair Coverage ......................      86.41 Perc

===============================================================================
Resolution & Completeness Statistics   (Cumulative and Friedel Pairs Averaged)
===============================================================================
Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     0.991          540      535        5
 23.01     0.550     0.993          703      698        5
 25.24     0.600     0.994          905      900        5
------------------------------------------------------------ ACTA Min. Res. ---
 27.51     0.650     0.996         1134     1129        5
 29.84     0.700     0.996         1413     1408        5
 32.21     0.750     0.995         1718     1709        9
 34.65     0.800     0.989         2067     2045       22
 36.32     0.833     0.963         2330     2243       87

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 .......          9

1,2 and 1,3 restraints were applied to the H-atoms on the water ligand
and solvent molecules.  Their H-atom positions were refined (see 
full text).
; 
 
_publ_section_exptl_prep 
; 
? 
; 
 
 
#end of refcif 
_cell_length_a                    12.2908(2)
_cell_length_b                    8.9941(2)
_cell_length_c                    7.6033(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      840.50(3)
 
_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 = C5 H7 N1 Ni1 O4 
# Dc =      1.61 Fooo =    504.00 Mu =     22.76 M =    203.82
# Found Formula = C4 H11 N1 Ni1 O7 
# Dc =      1.93 FOOO =    504.00 Mu =     23.18 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         9898
_cell_measurement_theta_min              3
_cell_measurement_theta_max             36
_cell_measurement_temperature          293
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.23 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_max           0.40 
 
_exptl_crystal_density_diffrn     1.927 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              504 
_exptl_absorpt_coefficient_mu     2.318 
 
# Sheldrick geometric approximatio 0.56 0.59 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'SADABS (Siemens, 1996)' 
_exptl_absorpt_correction_T_min   0.54 
_exptl_absorpt_correction_T_max   0.59 
_diffrn_measurement_device        'Bruker Kappa Apex2' 
_diffrn_measurement_device_type   'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71073
_diffrn_measurement_method        'φ & ω scans' 
 
# 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             15855 
_reflns_number_total              3763 
_diffrn_reflns_av_R_equivalents   0.019 
# Number of reflections with Friedels Law is 2243 
# Number of reflections without Friedels Law is 3763 
# Theoretical number of reflections is about 2037 
 
 
_diffrn_reflns_theta_min          2.806 
_diffrn_reflns_theta_max          36.318 
_diffrn_measured_fraction_theta_max 0.963 
 
_diffrn_reflns_theta_full         31.234 
_diffrn_measured_fraction_theta_full 0.995 
 
 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        12 
_reflns_limit_h_min               -20 
_reflns_limit_h_max               20 
_reflns_limit_k_min               0 
_reflns_limit_k_max               14 
_reflns_limit_l_min               0 
_reflns_limit_l_max               12 
 
_oxford_diffrn_Wilson_B_factor    1.41 
_oxford_diffrn_Wilson_scale       23.59 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    geom
 
_refine_diff_density_min          -0.36 
_refine_diff_density_max          0.40 
 
 
# 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          3763 
_refine_ls_number_restraints      9 
_refine_ls_number_parameters      137 
_oxford_refine_ls_R_factor_ref    0.0184 
_refine_ls_wR_factor_ref          0.0440 
_refine_ls_goodness_of_fit_ref    1.0457 
_refine_ls_shift/su_max           0.000266 
 
 
# The values computed from all data 
_oxford_reflns_number_all         3763 
_refine_ls_R_factor_all           0.0184 
_refine_ls_wR_factor_all          0.0440 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 3484 
_refine_ls_R_factor_gt            0.0164 
_refine_ls_wR_factor_gt           0.0396 
 
_refine_ls_abs_structure_Flack    0.015(7) 
_refine_ls_abs_structure_details  'Flack (1983), 1520 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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 0.06P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# 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. 
 
Siemens Industrial Automation, Inc (1996). 
SADABS: Area-Detector Absorption Correction;: Madison, WI. 
 
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 0.079183(9) 0.064017(12) 0.125103(19) 0.0180 1.0000 Uani . . . . . . . 
C1 C 0.26996(8) 0.22383(11) 0.20471(14) 0.0204 1.0000 Uani . . . . . . . 
C2 C 0.23999(7) 0.26487(11) 0.01616(14) 0.0191 1.0000 Uani . . . . . . . 
C3 C 0.16908(8) 0.40516(11) 0.01704(16) 0.0229 1.0000 Uani . . . . . . . 
C4 C 0.06247(7) 0.39756(10) 0.11798(16) 0.0195 1.0000 Uani . . . . . . . 
O1 O 0.20950(7) 0.12914(9) 0.28188(11) 0.0243 1.0000 Uani . . . . . . . 
O2 O 0.34892(7) 0.28689(10) 0.27604(13) 0.0315 1.0000 Uani . . . . . . . 
O3 O 0.01848(6) 0.27498(8) 0.15156(12) 0.0255 1.0000 Uani . . . . . . . 
O4 O 0.02200(7) 0.52029(9) 0.16253(13) 0.0306 1.0000 Uani . . . . . . . 
O5 O 0.13621(6) -0.15310(8) 0.11287(13) 0.0239 1.0000 Uani D . . . . . . 
O6 O -0.04313(8) 0.01242(11) -0.04959(18) 0.0430 1.0000 Uani D . . . . . . 
O7 O 0.09284(8) 0.21881(11) 0.58523(13) 0.0354 1.0000 Uani D . . . . . . 
N1 N 0.18236(7) 0.13926(10) -0.06428(13) 0.0206 1.0000 Uani . . . . . . . 
H11 H 0.2275 0.0707 -0.0942 0.0247 1.0000 Uiso . . . . . . . 
H12 H 0.1466 0.1680 -0.1553 0.0247 1.0000 Uiso . . . . . . . 
H21 H 0.3067 0.2847 -0.0505 0.0230 1.0000 Uiso . . . . . . . 
H31 H 0.2120 0.4849 0.0677 0.0274 1.0000 Uiso . . . . . . . 
H32 H 0.1518 0.4289 -0.1042 0.0274 1.0000 Uiso . . . . . . . 
H51 H 0.0891(13) -0.1967(18) 0.170(2) 0.0500 1.0000 Uiso D . . . . . . 
H52 H 0.1404(14) -0.2009(18) 0.0215(17) 0.0500 1.0000 Uiso D . . . . . . 
H61 H -0.0739(14) 0.0664(16) -0.120(2) 0.0500 1.0000 Uiso D . . . . . . 
H62 H -0.0636(15) -0.0720(12) -0.074(2) 0.0500 1.0000 Uiso D . . . . . . 
H71 H 0.1372(12) 0.202(2) 0.509(2) 0.0500 1.0000 Uiso D . . . . . . 
H72 H 0.0403(11) 0.171(2) 0.556(2) 0.0500 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 0.01917(5) 0.01482(5) 0.02000(6) -0.00066(5) 0.00121(5) 0.00046(4) 
C1 0.0209(4) 0.0196(4) 0.0208(5) 0.0006(3) -0.0009(3) 0.0013(3) 
C2 0.0195(3) 0.0192(4) 0.0187(4) 0.0014(3) 0.0031(3) 0.0013(3) 
C3 0.0253(4) 0.0183(4) 0.0250(5) 0.0062(3) 0.0061(4) 0.0031(3) 
C4 0.0231(4) 0.0161(3) 0.0195(4) 0.0026(3) 0.0030(3) 0.0034(3) 
O1 0.0292(3) 0.0232(3) 0.0207(4) 0.0050(3) -0.0045(3) -0.0043(3) 
O2 0.0307(4) 0.0328(4) 0.0311(5) 0.0017(4) -0.0092(3) -0.0084(3) 
O3 0.0249(3) 0.0154(3) 0.0360(5) -0.0004(3) 0.0100(3) 0.0009(2) 
O4 0.0378(4) 0.0157(3) 0.0382(5) 0.0010(3) 0.0175(4) 0.0058(3) 
O5 0.0256(3) 0.0196(3) 0.0266(4) 0.0014(3) 0.0042(3) 0.0017(2) 
O6 0.0406(5) 0.0252(4) 0.0632(7) 0.0001(4) -0.0297(5) 0.0003(4) 
O7 0.0424(5) 0.0366(4) 0.0271(5) -0.0014(4) -0.0052(3) 0.0023(4) 
N1 0.0244(3) 0.0202(4) 0.0172(4) -0.0022(3) 0.0015(3) 0.0026(3) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.19982(6) 
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 2.0756(8)    yes
Ni1 . C1 . 2.8161(10)    yes
Ni1 . C2 . 2.8028(10)    yes
Ni1 . O1 . 2.0808(8)    yes
Ni1 . O3 . 2.0487(7)    yes
Ni1 . O5 . 2.0768(7)    yes
Ni1 . O6 . 2.0590(10)    yes
Ni1 . N1 . 2.0346(9)    yes
C1 . C2 . 1.5255(15)    yes
C1 . O1 . 1.2734(12)    yes
C1 . O2 . 1.2482(12)    yes
C2 . C3 . 1.5335(14)    yes
C2 . N1 . 1.4670(13)    yes
C2 . H21 . 0.980    no
C3 . C4 . 1.5200(13)    yes
C3 . H31 . 0.970    no
C3 . H32 . 0.970    no
C4 . O3 . 1.2543(11)    yes
C4 . O4 . 1.2573(11)    yes
O5 . H51 . 0.822(9)    no
O5 . H52 . 0.818(9)    no
O6 . H61 . 0.813(9)    no
O6 . H62 . 0.821(9)    no
O7 . H71 . 0.813(9)    no
O7 . H72 . 0.807(9)    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 . C1 . 115.36(3)    yes
O4 3_545 Ni1 . C2 . 140.76(3)    yes
C1 . Ni1 . C2 . 31.50(3)    yes
O4 3_545 Ni1 . O1 . 93.95(4)    yes
C1 . Ni1 . O1 . 24.80(3)    yes
C2 . Ni1 . O1 . 56.29(3)    yes
O4 3_545 Ni1 . O3 . 83.16(3)    yes
C1 . Ni1 . O3 . 79.01(3)    yes
C2 . Ni1 . O3 . 71.88(3)    yes
O1 . Ni1 . O3 . 87.90(3)    yes
O4 3_545 Ni1 . O5 . 93.38(3)    yes
C1 . Ni1 . O5 . 102.04(3)    yes
C2 . Ni1 . O5 . 110.78(3)    yes
O1 . Ni1 . O5 . 91.75(3)    yes
O3 . Ni1 . O5 . 176.48(4)    yes
O4 3_545 Ni1 . O6 . 91.24(5)    yes
C1 . Ni1 . O6 . 149.50(4)    yes
C2 . Ni1 . O6 . 118.00(4)    yes
O1 . Ni1 . O6 . 174.29(4)    yes
O3 . Ni1 . O6 . 90.35(4)    yes
O4 3_545 Ni1 . N1 . 170.75(3)    yes
C1 . Ni1 . N1 . 57.54(3)    yes
C2 . Ni1 . N1 . 30.34(3)    yes
O1 . Ni1 . N1 . 80.33(4)    yes
O3 . Ni1 . N1 . 89.34(3)    yes
O5 . Ni1 . O6 . 90.32(4)    yes
O5 . Ni1 . N1 . 94.06(3)    yes
O6 . Ni1 . N1 . 94.21(5)    yes
Ni1 . C1 . C2 . 73.77(5)    yes
Ni1 . C1 . O1 . 43.27(5)    yes
C2 . C1 . O1 . 117.00(9)    yes
Ni1 . C1 . O2 . 166.61(8)    yes
C2 . C1 . O2 . 119.09(9)    yes
O1 . C1 . O2 . 123.88(10)    yes
C1 . C2 . Ni1 . 74.73(5)    yes
C1 . C2 . C3 . 109.40(8)    yes
Ni1 . C2 . C3 . 97.37(5)    yes
C1 . C2 . N1 . 108.78(8)    yes
Ni1 . C2 . N1 . 44.47(4)    yes
C3 . C2 . N1 . 111.17(8)    yes
C1 . C2 . H21 . 109.2    no
Ni1 . C2 . H21 . 149.3    no
C3 . C2 . H21 . 109.2    no
N1 . C2 . H21 . 109.2    no
C2 . C3 . C4 . 117.07(8)    yes
C2 . C3 . H31 . 107.5    no
C4 . C3 . H31 . 107.5    no
C2 . C3 . H32 . 107.5    no
C4 . C3 . H32 . 107.5    no
H31 . C3 . H32 . 109.5    no
C3 . C4 . O3 . 120.92(8)    yes
C3 . C4 . O4 . 115.95(8)    yes
O3 . C4 . O4 . 123.12(9)    yes
C1 . O1 . Ni1 . 111.93(7)    yes
C4 . O3 . Ni1 . 129.58(6)    yes
C4 . O4 . Ni1 3_555 127.81(7)    yes
Ni1 . O5 . H51 . 100.8(13)    no
Ni1 . O5 . H52 . 123.6(14)    no
H51 . O5 . H52 . 103.9(9)    no
Ni1 . O6 . H61 . 128.8(12)    no
Ni1 . O6 . H62 . 125.3(12)    no
H61 . O6 . H62 . 105.2(9)    no
H71 . O7 . H72 . 103.6(9)    no
C2 . N1 . Ni1 . 105.19(6)    yes
C2 . N1 . H11 . 110.5    no
Ni1 . N1 . H11 . 110.5    no
C2 . N1 . H12 . 110.5    no
Ni1 . N1 . H12 . 110.5    no
H11 . N1 . H12 . 109.5    no
