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)cobalt(II) — methanol (1:2), Co2(C32H52N6O2)(NCS)2 · 2CH3OH
Ying-Yin Jiang; Dao-Cheng Xia; Jian-Fang Ma; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 49–; doi:

data_8102583
_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)cobalt(II)
 --- methanol (1:2), Co2(C32H52N6O2)(NCS)2 &#x00B7; 2CH3OH
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              49
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C34 H52 Co2 N8 O2 S2, 2(CH3 OH)'
_chemical_formula_sum            'C36 H60 Co2 N8 O4 S2'
_chemical_formula_weight         842.84
_chemical_melting_point          ?
_chemical_name_common
;
[\m-13,27-di-<i>tert</i>-butyl-3,6,9,17,20,23-hexaazatri- cyclo
[23,3,1,1^11,15^]triaconta-1(28),11,13,15
(30),25,26-hexaene-29,30-diolato[\k^5^<i>N^3^</i>,<i>N^6^</i>,<i>N^9^</i>,\
<i>O^29^</i>,<i>O^30^</i>:\k^5^<i>N^17^</i>,<i>N^20^</i>,<i>N^23^</i>,\
<i>O^29^</i>,<i>O^30^</i>]bis(thiocyanato-\kN)cobalt(II)--methanol (1:2)
;
_chemical_name_systematic
;
[\m-13,27-di-<i>tert</i>-butyl-3,6,9,17,20,23-hexaazatri- cyclo
[23,3,1,1^11,15^]triaconta-1(28),11,13,15
(30),25,26-hexaene-29,30-diolato[\k^5^<i>N^3^</i>,<i>N^6^</i>,<i>N^9^</i>,\
<i>O^29^</i>,<i>O^30^</i>:\k^5^<i>N^17^</i>,<i>N^20^</i>,<i>N^23^</i>,\
<i>O^29^</i>,<i>O^30^</i>]bis(thiocyanato-\kN)cobalt(II)---methanol (1:2)
;
_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
_cell_angle_alpha                77.44(3)
_cell_angle_beta                 79.73(3)
_cell_angle_gamma                82.19(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4580(17)
_cell_length_b                   10.448(2)
_cell_length_c                   12.553(3)
_cell_measurement_reflns_used    4780
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.470
_cell_measurement_theta_min      3.10
_cell_volume                     1059.9(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO(Rigaku, 1998)[4]'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)[5]'
_computing_structure_solution    'SHELXS-97 '
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10383
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Higashi,T (1995) Program for absorption correction. 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.527
_exptl_crystal_size_mid          0.424
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4780
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.3510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                3742
_reflns_number_total             4780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2801.cff
_cod_data_source_block           yy
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-09-11

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_database_code               8102583