Modulation of the architectures and magnetic dynamics in pseudotetrahedral cobalt(II) complexes
Zhou, Yuting; Li, Yuzhu; Xi, Jing; Qin, Yuanyuan; Cen, Peipei; Zhang, Yi-Quan; Guo, Yan; Ding, Yi; Liu, Xiangyu; Dalton Transactions  (2022) –; doi:10.1039/D2DT01047J

data_7710129
_publ_section_title
;
 Modulation of the architectures and magnetic dynamics in
 pseudotetrahedral cobalt(II) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01047J
_journal_year                    2022
_chemical_formula_moiety         'C90 H98 Cl2 Co2 N4, 2(C6 H14)'
_chemical_formula_sum            'C102 H126 Cl2 Co2 N4'
_chemical_formula_weight         1596.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                112.016(6)
_cell_angle_beta                 106.072(6)
_cell_angle_gamma                104.125(6)
_cell_formula_units_Z            1
_cell_length_a                   13.519(2)
_cell_length_b                   13.643(2)
_cell_length_c                   14.754(2)
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      26.418
_cell_measurement_theta_min      2.421
_cell_volume                     2231.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         2.422
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1212 before and 0.0453 after correction. The Ratio of minimum to maximum transmission is 0.9166. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0487P)^2^+1.9811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7372
_reflns_number_total             9144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01047j2.cif
_cod_data_source_block           guoyan20181122
_cod_original_cell_volume        2231.7(6)
_cod_database_code               7710129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=
 Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=FVAR(1)
3.a Riding coordinates:
 C46(H46A,H46B,H46C,H46D,H46E,H46F)
3.b Ternary CH refined with riding coordinates:
 C35(H35), C44(H44), C5(H5), C13(H13)
3.c Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C50(H50A,H50B), C51(H51A,H51B), C48(H48A,H48B), C47A(H47C,
 H47D), C48A(H48C,H48D)
3.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C29(H29), C27(H27), C8(H8), C38(H38), C17(H17), C33(H33), C10(H10),
 C25(H25), C24(H24), C21(H21), C40(H40), C26(H26), C18(H18), C30(H30), C9(H9),
 C39(H39), C20(H20), C32(H32), C31(H31), C19(H19)
3.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C43(H43A,H43B,H43C), C36(H36A,H36B,H36C), C34(H34A,H34B,
 H34C), C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C45(H45A,H45B,H45C), C6(H6A,H6B,
 H6C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              31031
_olex2_submission_special_instructions 'No special instructions were received'