Structural and transport properties of neutral radical crystals of Co(III)(tmp)(CN)2 (tmp = 5,10,15,20-tetramethylporphyrinato) and the CN-bridged polymer [Co(III)(tmp)(CN)]n.
Kurokawa, Masashi; Jose-Larong, Judy Fe F; Hasegawa, Hiroyuki; Takahashi, Yukihiro; Harada, Jun; Inabe, Tamotsu; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4422–4429; doi:10.1039/c6dt04418b

data_7042334
_publ_section_title
;
 Structural and transport properties of neutral radical crystals of
 Co(III)(tmp)(CN)2 (tmp = 5,10,15,20-tetramethylporphyrinato) and the
 CN-bridged polymer [Co(III)(tmp)(CN)]n.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4422
_journal_page_last               4429
_journal_paper_doi               10.1039/c6dt04418b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C26 H20 Co N6'
_chemical_formula_sum            'C26 H20 Co N6'
_chemical_formula_weight         475.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                89.409(4)
_cell_angle_beta                 81.068(4)
_cell_angle_gamma                76.910(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6078(17)
_cell_length_b                   9.3943(18)
_cell_length_c                   13.337(3)
_cell_measurement_reflns_used    5401
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.512
_cell_measurement_theta_min      2.227
_cell_volume                     1037.4(4)
_computing_cell_refinement       'Bruker SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEXII Ultra'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30578
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         1.546
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.949527
_exptl_absorpt_correction_T_min  0.748417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0793 before and 0.0535 after correction.
 The Ratio of minimum to maximum transmission is 0.79.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0890 before and 0.0612 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 30578 reflections, Rint = 0.0867
 (15683 with I > 3sig(I), Rint = 0.0661)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.6093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3294
_reflns_number_total             4755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04418b2.cif
_cod_data_source_block           Co-CN2tmp_100K
_cod_depositor_comments
'Adding full bibliography for 7042332--7042335.cif.'
_cod_original_cell_volume        1037.3(4)
_cod_database_code               7042334
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              82436
_olex2_submission_special_instructions 'No special instructions were received'