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_1542327
_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_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             2014-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_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                   18.967(3)
_cell_length_b                   8.6864(12)
_cell_length_c                   33.532(5)
_cell_measurement_reflns_used    5146
_cell_measurement_temperature    130.15
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.23
_cell_volume                     5524.6(14)
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_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  0.1147
_diffrn_reflns_av_unetI/netI     0.1092
_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            54108
_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         26.022
_diffrn_reflns_theta_min         2.147
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0798 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.8425.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue/black
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       needle
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.437(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         10889
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7127
_reflns_number_total             10889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03547c2.cif
_cod_data_source_block           pna21
_cod_original_cell_volume        5524.8(13)
_cod_database_code               1542327
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(18) 0.437(18)
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), C27(H27), C28(H28), C29(H29), C30(H30), 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              93740
_olex2_submission_special_instructions 'No special instructions were received'