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_1542328
_publ_section_title
;
 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_MeCN
_chemical_name_systematic
'Cobalt(II) bis(2,2';6',2"-terpyridine) tetracyanoquinodimethanide mono 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             2015-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-19 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                   19.074(6)
_cell_length_b                   8.705(3)
_cell_length_c                   33.611(10)
_cell_measurement_reflns_used    6560
_cell_measurement_temperature    190
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      2.22
_cell_volume                     5581(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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0928
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            55562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0780 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.9188.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.489(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         11002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0167P)^2^+2.3072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8231
_reflns_number_total             11002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03547c2.cif
_cod_data_source_block           190k_a
_cod_database_code               1542328
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8 0.2
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C59(H59), C60(H60),
 C62(H62), C63(H63), C35(H35), C36(H36), C38(H38), C39(H39), C47(H47), C48(H48),
  C50(H50), C51(H51)
3.b Idealised Me refined as rotating group:
 C68(H68a,H68b,H68c)
;
_shelx_res_checksum              29408
_olex2_submission_special_instructions 'No special instructions were received'