Crystal structure of [m-13,27-di-tert-butyl-3,6,9,17,20,23-hexaazatricyclo[23,3,1,111,15]triaconta-1(28),11,13,15 (30),25,26-hexaene-29,30-diolato-[k5N3,N6,N9,O29,O30:k5N17,N20,N23,O29,O30]bis(thiocyanato-kN)nickel(II) — methanol (1:0.5), Ni2(C32H52N6O2)(NCS)2 · 0.5CH3OH
Ying-Yin Jiang; Dao-Cheng Xia; Jian-Fang Ma; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 693–; doi:

data_8102541
_publ_section_title
;
 Crystal structure of
 [m-13,27-di-tert-butyl-3,6,9,17,20,23-hexaazatricyclo[23,3,1,111,15]triaconta-1(28),11,13,15
 (30),25,26-hexaene-29,30-diolato-[k5N3,N6,N9,O29,O30:k5N17,N20,N23,O29,O30]bis(thiocyanato-kN)nickel(II)
 --- methanol (1:0.5), Ni2(C32H52N6O2)(NCS)2 &#x00B7; 0.5CH3OH
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              693
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C34 H52 N8 Ni2 O2 S2, 0.5(C H4 O)'
_chemical_formula_sum            'C34.5 H54 N8 Ni2 O2.5 S2'
_chemical_formula_weight         802.40
_chemical_melting_point          ?
_chemical_name_common
;
Crystal structure of
 [\m-13,27-ditertbutyl-3,6,9,17,20,23-hexaazatricyclo
 [23,3,1,111,15]triaconta-1(28),11,13,15
 (30),25,26-hexaene-29,30-diolato[\k5N3,N6,N9,O29,O30
 :\k5N17,N20,N23,O29,O30]bis(thiocyanato-\kN)nickel(II)
;
_chemical_name_systematic
;
  Crystal structure of [\m-13,27-ditertbutyl-3,6,9,17,20,23-hexaazatricyclo
 [23,3,1,111,15]triaconta-1(28),11,13,15
 (30),25,26-hexaene-29,30-diolato[\k5N3,N6,N9,O29,O30
 :\k5N17,N20,N23,O29,O30]bis(thiocyanato-\kN)nickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-08-26 # Formatted by publCIF
;
_cell_angle_alpha                77.422(9)
_cell_angle_beta                 79.470(9)
_cell_angle_gamma                81.725(9)
_cell_formula_units_Z            1
_cell_length_a                   8.5140(10)
_cell_length_b                   10.4120(11)
_cell_length_c                   12.5710(14)
_cell_measurement_reflns_used    4890
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.110
_cell_measurement_theta_min      3.09
_cell_volume                     1063.0(2)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis [4]'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 [5]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9726
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         4.46
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Oxford Diffraction: CrysAlis [4].'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             425
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                3712
_reflns_number_total             4890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2753.cff
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1 '
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C34.50 H54 N8 Ni2 O2.50 S2'
_cod_database_code               8102541