Crystal structure of [3,7,11,18,22,26-hexaaza-tricyclo[26.2.2.213,16]-tetratriaconta-1(31),13(34),14,16(33),28(32),29-hexaene]dinickel tetrachloride — methanol — water (1:1:1), Ni2(C28H46N6)Cl4 · CH3OH · H2O
Hua Wu; Dao-Cheng Xia; Hai-Yan Liu; Hong-Ye Bai; Jian-Fang Ma; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 695–; doi:

data_8102572
_publ_section_title
;
 Crystal structure of
 [3,7,11,18,22,26-hexaaza-tricyclo[26.2.2.213,16]-tetratriaconta-1(31),13(34),14,16(33),28(32),29-hexaene]dinickel
 tetrachloride --- methanol --- water (1:1:1), Ni2(C28H46N6)Cl4
 &#x00B7; CH3OH &#x00B7; H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              695
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C28 H46 Cl4 N6 Ni2, C H4 O, H2 O'
_chemical_formula_sum            'C29 H51 Cl4 N6 Ni2 O2'
_chemical_formula_weight         774.98
_chemical_melting_point          ?
_chemical_name_systematic
;
[3,7,11,18,22,26-hexaazatricyclo[26.2.2.2^13,16^] tetratriaconta-
1(31),13(34),14,16(33), 28(32),29-hexaene] dinickel tetra-chloride
methanol monhydrate
;
_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                 106.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.928(2)
_cell_length_b                   15.437(3)
_cell_length_c                   11.621(2)
_cell_measurement_reflns_used    4229
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1878.8(7)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17661
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Abscor (Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.9845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                3302
_reflns_number_total             4229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2789.cff
_cod_data_source_block           p21n
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-02-05

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 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               8102572