Crystal structure of bis[(diaquahydroxy-(1,12,15-triaza-3,4:9,10-dibenzo-5,8-dioxacycloheptadecane-k3N,N',N'')nickel(II)] benzene-1,4-dicarboxylate heptahydrate, [Ni(H2O)2(OH)(C20H27N3O2)]2[C8H4O4] · 7H2O
Hong-Ye Bai; Ying-Ying Liu; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 529–; doi:

data_8102766
_publ_section_title
;
 Crystal structure of
 bis[(diaquahydroxy-(1,12,15-triaza-3,4:9,10-dibenzo-5,8-dioxacycloheptadecane-k3N,N',N'')nickel(II)]
 benzene-1,4-dicarboxylate heptahydrate,
 [Ni(H2O)2(OH)(C20H27N3O2)]2[C8H4O4] &#x00B7; 7H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              529
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C40 H64 N6 Ni2 O10, C8 H4 O4, 7(H2 O)'
_chemical_formula_sum            'C48 H82 N6 Ni2 O21'
_chemical_formula_weight         1196.62
_chemical_name_systematic
;
bis[(triaqua-(1,12,15-triaza-
3,4:9,10-dibenzo-5,8-dioxacyclo-heptadecane-<i>\k</i>^3^N,N',N'')
nickel (II)] (benzene-1,4-dicarboxylate) heptahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.445(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.130(4)
_cell_length_b                   11.475(3)
_cell_length_c                   19.767(6)
_cell_measurement_reflns_used    6565
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2884.1(15)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27282
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi,T (1995) Program for absorption correction. 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+2.1076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                5148
_reflns_number_total             6565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3063.cff
_cod_data_source_block           a
_cod_depositor_comments
;
 Marking atom disorder assemblies after consulting the original publication.
 Atoms 'O3' and 'O3'' were marked as belonging to disorder groups '1' and '2'
 of disorder assembly A. Atoms 'O4' and 'O4'' were marked as belonging to
 disorder groups '1' and '2' of disorder assembly B.

 Antanas Vaitkus,
 2017-09-11

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        2884.1(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8102766