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_7042332
_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, C24 H20 P, 0.5(C3 H6 O), O'
_chemical_formula_sum            'C51.5 H45 Co N6 O1.5 P'
_chemical_formula_weight         861.83
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                65.6430(10)
_cell_angle_beta                 69.3160(10)
_cell_angle_gamma                77.5240(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0125(9)
_cell_length_b                   13.6844(10)
_cell_length_c                   14.8622(11)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.475
_cell_measurement_theta_min      2.345
_cell_volume                     2075.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         1.808
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1151 before and 0.0297 after correction. The Ratio of minimum to maximum transmission is 0.9501. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9517
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0516P)^2^+1.9609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8825
_reflns_number_total             9517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04418b2.cif
_cod_data_source_block           Co-tmp-CN2_TPP_100K
_cod_depositor_comments
'Adding full bibliography for 7042332--7042335.cif.'
_cod_original_formula_sum        'C51.50 H45 Co N6 O1.50 P'
_cod_database_code               7042332
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.868
_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. Same fragment restrains
{O1A, C1A, C2A, C3A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1B, C1B, C2B, C3B}
3. Others
 Fixed Sof: O1A(0.25) C1A(0.25) C2A(0.25) H2A1(0.25) H2A2(0.25) H2A3(0.25)
 C3A(0.25) H3A1(0.25) H3A2(0.25) H3A3(0.25) O1B(0.25) C1B(0.25) C2B(0.25)
 H2B1(0.25) H2B2(0.25) H2B3(0.25) C3B(0.25) H3B1(0.25) H3B2(0.25) H3B3(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C2A(H2A1,H2A2,H2A3), C3A(H3A1,H3A2,H3A3), C2B(H2B1,H2B2,H2B3), C3B(H3B1,
 H3B2,H3B3)
;
_shelx_res_checksum              72369
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'