A cobalt(ii) spin-crossover compound with partially charged TCNQ radicals and an anomalous conducting behavior
Zhang, Xuan; Wang, Zhao-Xi; Xie, Haomiao; Li, Ming-Xing; Woods, Toby J.; Dunbar, Kim R.; Chem. Sci. 7 (2016) 1569–; doi:10.1039/C5SC03547C

data_1542323
_publ_section_title
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 A cobalt(ii) spin-crossover compound with partially charged TCNQ radicals
 and an anomalous conducting behavior
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1569
_journal_paper_doi               10.1039/C5SC03547C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C30 H22 Co N6, 3(C12 H4 N4), C2 H3 N'
_chemical_formula_sum            'C68 H37 Co N19'
_chemical_formula_weight         1179.09
_chemical_name_common            Co(terpy)2(TCNQ)3(CH3CN)
_chemical_name_systematic
'Cobalt(II) bis(2,2?:6?,2??-terpyridine) tri-7,7,8,8-tetracyanoquinodimethanide acetonitrile'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-02-12 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9411(10)
_cell_length_b                   8.6917(4)
_cell_length_c                   33.5158(17)
_cell_measurement_reflns_used    8992
_cell_measurement_temperature    100
_cell_measurement_theta_max      16.525
_cell_measurement_theta_min      2.164
_cell_volume                     5517.7(5)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.1046
_diffrn_reflns_av_unetI/netI     0.1007
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            77611
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.150
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.8653.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       needle
_exptl_crystal_F_000             2420
_exptl_crystal_preparation
'Magnetic properties, electrical conducting properties'
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.486(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         14467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0545P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                10980
_reflns_number_total             14467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03547c2.cif
_cod_data_source_block           100
_cod_database_code               1542323
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.946
_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:
 C51(H51), C15(H15), C38(H38), C9(H9), C39(H39), C7(H7), C36(H36), C63(H63),
 C50(H50), C47(H47), C8(H8), C6(H6), C62(H62), C30(H30), C48(H48), C35(H35),
 C60(H60), C13(H13), C29(H29), C2(H2), C12(H12), C14(H14), C27(H27), C4(H4),
 C59(H59), C25(H25), C3(H3), C23(H23), C19(H19), C17(H17), C22(H22), C28(H28),
 C18(H18), C24(H24)
2.b Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              77177
_olex2_submission_special_instructions 'No special instructions were received'