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_7042333
_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         '0.25(C100 H80 Co4 N20), C3 H6 O'
_chemical_formula_sum            'C28 H26 Co N5 O'
_chemical_formula_weight         507.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-31
_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                90
_cell_angle_beta                 114.655(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7053(17)
_cell_length_b                   19.130(3)
_cell_length_c                   11.7373(17)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.236
_cell_measurement_theta_min      2.186
_cell_volume                     2388.6(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0985
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52132
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.958251
_exptl_absorpt_correction_T_min  0.848790
_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 0.0706 before and 0.0579 after correction.
 The Ratio of minimum to maximum transmission is 0.89.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 52132 reflections, Rint = 0.0985
 (19464 with I > 3sig(I), Rint = 0.0683)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 3201 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         11380
_refine_ls_number_restraints     719
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+4.1082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8733
_reflns_number_total             11380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04418b2.cif
_cod_data_source_block           polymer_acetone_100K1
_cod_depositor_comments
'Adding full bibliography for 7042332--7042335.cif.'
_cod_original_cell_volume        2388.7(6)
_cod_database_code               7042333
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.82(5) 0.15(3) 0.03(3) 0.00(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O1A, C51A, C52, C53} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1B, C51B, C52, C53}
{O1A, C51A, C52, C53} sigma for 1-2: 0.02, 1-3: 0.04
as
{O2, C54, C55, C56}
5. Others
 Sof(O1B)=Sof(C51B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(H53D)=Sof(H53E)=
 Sof(H53F)=1-FVAR(1)
 Sof(O1A)=Sof(C51A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C27(H27), C28(H28), C32(H32), C33(H33), C37(H37), C38(H38), C42(H42), C43(H43)
6.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C52(H52A,H52B,H52C), C52(H52D,H52E,H52F), C53(H53A,H53B,H53C),
 C53(H53D,H53E,H53F), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              27379
_olex2_submission_special_instructions 'No special instructions were received'