Exploring a prototype for cooperative structural phase transition in cobalt(II) spin crossover compounds.
Deng, Yi-Fei; Wang, Yi-Nuo; Zhao, Xin-Hua; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 699–705; doi:10.1039/d3dt03529h

data_7714535
_publ_section_title
;
 Exploring a prototype for cooperative structural phase transition in
 cobalt(II) spin crossover compounds.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              699
_journal_page_last               705
_journal_paper_doi               10.1039/d3dt03529h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H32 Co N6, 2(Cl O4), H2 O, 2(C H4 O)'
_chemical_formula_sum            'C40 H42 Cl2 Co N6 O11'
_chemical_formula_weight         912.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.102(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8068(12)
_cell_length_b                   20.3436(17)
_cell_length_c                   14.7359(13)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.22
_cell_volume                     4136.2(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23511
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.738
_diffrn_reflns_theta_max         24.738
_diffrn_reflns_theta_min         2.434
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1316 before and 0.0794 after correction.
The Ratio of minimum to maximum transmission is 0.7947.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_refine_diff_density_max         1.157
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+15.5138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6066
_reflns_number_total             7031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03529h2.cif
_cod_data_source_block           150k
_cod_depositor_comments
'Adding full bibliography for 7714535--7714539.cif.'
_cod_database_code               7714535
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 O11-C40
 1.52 with sigma of 0.02
 C39-O10
 1.52 with sigma of 0.02
 C40-O11
 1.6 with sigma of 0.02
 O10-C39
 1.6 with sigma of 0.02
2. Rigid bond restraints
 C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1A) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) = Uanis(C12)
4. Others
 Sof(O1B)=1-FVAR(1)
 Sof(O1A)=FVAR(1)
5.a Free rotating group:
 O9(H9A,H9B)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
5.e Idealised tetrahedral OH refined as rotating group:
 O10(H10A), O11(H11A)
;
_shelx_res_checksum              25979
_olex2_submission_special_instructions 'No special instructions were received'