Structural distortions of the spin-crossover material [Co(pyterpy)2](TCNQ)2 mediated by supramolecular interactions
Xuan Zhang; Haomiao Xie; Maria Ballesteros-Rivas; Zhao-Xi Wang; Kim R. Dunbar; Journal of Materials Chemistry C 3 (2015) 9292–9298; doi:10.1039/C5TC01851J

data_7234428
_publ_section_title
;
 Structural distortions of the spin-crossover material
 [Co(pyterpy)2](TCNQ)2 mediated by supramolecular interactions
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              9292
_journal_page_last               9298
_journal_paper_doi               10.1039/C5TC01851J
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C40 H28 Co N8, 4(F2.58 P0.5), 1.69(F1)'
_chemical_formula_sum            'C40 H28 Co F12 N8 P2'
_chemical_formula_weight         969.57
_chemical_name_common            Co(pyterpy)2(PF6)2
_chemical_name_systematic
;  
Cobalt(II) bis-(4?-(4???-pyridyl)- 2,2?:6?,2??-terpyridine) hexafluorophosphate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.888(12)
_cell_length_b                   8.888(12)
_cell_length_c                   57.91(8)
_cell_measurement_reflns_used    3086
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.32
_cell_volume                     4575(11)
_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      300.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1007
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            22459
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.676
_diffrn_reflns_theta_min         1.407
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0962 before and 0.0835 after correction.
The Ratio of minimum to maximum transmission is 0.8512.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.902
_refine_ls_R_factor_all          0.1894
_refine_ls_R_factor_gt           0.1643
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4576
_refine_ls_wR_factor_ref         0.4708
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1646
_reflns_number_total             2177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2015-3-9292.cif
_cod_data_source_block           4-300K
_cod_original_cell_volume        4575(13)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7234428
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.02
 F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F1-F6
 with sigma of 0.02
 F2-F3 \\sim F2-F4 \\sim F2-F5 \\sim F2-F6
 with sigma of 0.02
 F6-F1 \\sim F6-F2 \\sim F6-F3 \\sim F6-F4
 with sigma of 0.02
 F5-F1 \\sim F5-F2 \\sim F5-F3 \\sim F5-F4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(F2) = Uiso(F3) = Uiso(F5) = Uiso(F6) = Uiso(F1)
Uiso(F4) = Uiso(F4A)
4. Others
 Sof(F4A)=0.5*(1-FVAR(2))
 Sof(F4)=0.5*FVAR(2)
 Fixed Sof: P1(0.5) F6(0.5) F2(0.5) F1(0.5) F3(0.5) F5(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C2(H2), C7(H7), C6(H6), C10(H10), C11(H11)
;
_shelx_res_checksum              21673