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_7710130
_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         'C50 H54 Cl Co N3, 0.5(C7 H8), 0.5(C6 H14)'
_chemical_formula_sum            'C56.5 H65 Cl Co N3'
_chemical_formula_weight         880.49
_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             2021-01-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                102.736(4)
_cell_angle_beta                 99.487(4)
_cell_angle_gamma                100.369(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4237(12)
_cell_length_b                   12.6248(16)
_cell_length_c                   22.087(3)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      2.16
_cell_volume                     2463.3(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            115432
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.221
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11211
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8732
_reflns_number_total             11211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01047j2.cif
_cod_data_source_block           lyzco9
_cod_original_cell_volume        2463.3(5)
_cod_original_formula_sum        'C56.50 H65 Cl Co N3'
_cod_database_code               7710130
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.949
_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
2. Restrained distances
 C63-C62 = C62-C61 = C61-C60 = C60-C59 = C59-C58
 1.52 with sigma of 0.02
 C56-C55 = C54-C53 = C53-C52
 1.38 with sigma of 0.02
 C51-C56 = C51-C52 = C55-C54
 1.39 with sigma of 0.02
 C57-C51
 1.51 with sigma of 0.02
 C62-C60 = C61-C59
 2.54 with sigma of 0.04
 C63-C61 = C60-C58
 2.53 with sigma of 0.04
 C51-C55
 2.42 with sigma of 0.04
 C57-C56 = C57-C52
 2.52 with sigma of 0.04
 C55-C53 = C54-C52
 2.4 with sigma of 0.04
 C51-C53
 2.41 with sigma of 0.04
 C56-C54
 2.39 with sigma of 0.04
 C63-C62 \\sim C62-C61 \\sim C61-C60 \\sim C60-C59 \\sim C59-C58
 with sigma of 0.02
 C63-C61 \\sim C61-C59 \\sim C62-C60 \\sim C60-C58
 with sigma of 0.04
 C51-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C53 \\sim C53-C52 \\sim C52-C51
 with sigma of 0.02
 C51-C53 \\sim C51-C55 \\sim C52-C54 \\sim C56-C52 \\sim C55-C53 \\sim C56-C54
 with sigma of 0.04
 C57-C52 \\sim C57-C56
 with sigma of 0.04
3. Restrained planarity
 C51, C52, C53, C54, C55, C56, C57
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C57 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C63 \\sim
C62 \\sim C61 \\sim C60 \\sim C59 \\sim C58: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C57) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C52, C53, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5)
 C55(0.5) H55(0.5) C56(0.5) H56(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
7.a Riding coordinates:
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C63(H63A,H63B,H63C)
7.b Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C40(H40), C43(H43)
7.c Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
7.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C)
;
_shelx_res_checksum              67941
_olex2_submission_special_instructions 'No special instructions were received'