Spin transition triggered by desorption of crystal solvents for a two-dimensional cobalt(ii) complex with hydrogen bonding.
Kanetomo, Takuya; Inokuma, Kiwamu; Naoi, Yuya; Enomoto, Masaya; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11243–11248; doi:10.1039/d1dt01934a

data_7707846
_publ_section_title
;
 Spin transition triggered by desorption of crystal solvents for a
 two-dimensional cobalt(ii) complex with hydrogen bonding.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11243
_journal_page_last               11248
_journal_paper_doi               10.1039/d1dt01934a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C46 H58 Co N10 O4, 2(C24 H20 B), C3 H6 O'
_chemical_formula_sum            'C97 H104 B2 Co N10 O5'
_chemical_formula_weight         1570.45
_chemical_melting_point          478
_chemical_name_systematic        '[Co(5tpybNOH)2](BPh4)2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-02 deposited with the CCDC.	2021-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3784(4)
_cell_length_b                   19.8247(3)
_cell_length_c                   22.6637(4)
_cell_measurement_reflns_used    17645
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      76.4090
_cell_measurement_theta_min      2.9430
_cell_volume                     10503.9(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38333
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.546
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              PhotonJet-S
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_description       block
_exptl_crystal_F_000             3332
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/n-hexane'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 5903 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.134(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         18180
_refine_ls_number_restraints     542
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+7.5524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1706
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.659
_reflns_number_gt                16546
_reflns_number_total             18180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01934a1.cif
_cod_data_source_block           co5tpybnoh_2_sq
_cod_depositor_comments          'Adding full bibliography for 7707846.cif.'
_cod_database_code               7707846
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5864(14)
 0.4136(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 N10-C37 \\sim N10A-C37
 with sigma of 0.02
 C14-N5 \\sim C14-N5A
 with sigma of 0.02
 N5-C20 \\sim N5A-C20A
 with sigma of 0.02
 C20-C22 \\sim C20A-C21A
 with sigma of 0.02
 C20-C23 \\sim C20A-C22A
 with sigma of 0.02
 C20-C21 \\sim C20A-C23A
 with sigma of 0.02
 C14-C20 \\sim C14-C20A
 with sigma of 0.04
 N5-C22 \\sim N5A-C21A
 with sigma of 0.04
 N5-C23 \\sim N5A-C22A
 with sigma of 0.04
 N5-C21 \\sim N5A-C23A
 with sigma of 0.04
 C22-C23 \\sim C21A-C22A
 with sigma of 0.04
 C22-C21 \\sim C21A-C23A
 with sigma of 0.04
 C23-C21 \\sim C22A-C23A
 with sigma of 0.04
 N10-C43 \\sim N10A-C43A
 with sigma of 0.02
 C43-C44 \\sim C43A-C45A
 with sigma of 0.02
 C43-C45 \\sim C43A-C44A
 with sigma of 0.02
 C43-C46 \\sim C43A-C46A
 with sigma of 0.02
 N10-C44 \\sim N10A-C45A
 with sigma of 0.04
 N10-C45 \\sim N10A-C44A
 with sigma of 0.04
 N10-C46 \\sim N10A-C46A
 with sigma of 0.04
 C37-C43 \\sim C37-C43A
 with sigma of 0.04
 C44-C45 \\sim C45A-C44A
 with sigma of 0.04
 C44-C46 \\sim C45A-C46A
 with sigma of 0.04
 C45-C46 \\sim C44A-C46A
 with sigma of 0.04
 N10-O4 \\sim N10A-O4A
 with sigma of 0.02
 O4-C37 \\sim O4A-C37
 with sigma of 0.04
 N5-O2 \\sim N5A-O2A
 with sigma of 0.02
 C14-O2 \\sim C14-O2A
 with sigma of 0.04
 O2-C20 \\sim O2A-C20A
 with sigma of 0.04
 O4-C43 \\sim O4A-C43A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
N5 \\sim O2 \\sim C20 \\sim C21 \\sim C23A \\sim C20A \\sim C22A \\sim N5A
\\sim C22 \\sim C21A \\sim O2A \\sim C23: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
N10A \\sim N10 \\sim O4 \\sim O4A \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim
C44A \\sim C43A \\sim C45A \\sim C46A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
C1A \\sim O7 \\sim C1B \\sim C1C: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C20, C22, C23, C21, C23A, C20A, C21A, C22A, O2A, N5, O2, N5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, O4, C43, C44, C45, C46, N10A, O4A, C44A, C43A, C45A, C46A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, O7, C1A, C1C, H1AA, H1AB, H1AC, H1CA, H1CB, H1CC
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N10A)=Sof(O4A)=Sof(H4A)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C43A)=
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46A)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=1-FVAR(1)
 Sof(N10)=Sof(O4)=Sof(H4)=Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 FVAR(1)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C20A)=Sof(C21A)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(N5A)=Sof(O2A)=
 Sof(H2AA)=1-FVAR(2)
 Sof(N5)=Sof(O2)=Sof(H2A)=Sof(C20)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 FVAR(2)
7.a Free rotating group:
 C43(C44,C45,C46), C20(C22,C23,C21)
7.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C21(H21A,H21B,H21C), C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F),
 C46A(H46D,H46E,H46F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F), C22A(H22D,
 H22E,H22F), C1A(H1AA,H1AB,H1AC), C1C(H1CA,H1CB,H1CC)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C15(H15), C70(H70), C80(H80), C91(H91), C90(H90), C64(H64), C73(H73),
  C12(H12), C13(H13), C86(H86), C69(H69), C28(H28), C92(H92), C25(H25),
 C54(H54), C84(H84), C72(H72), C55(H55), C2(H2), C5(H5), C62(H62), C30(H30),
 C85(H85), C9(H9), C76(H76), C32(H32), C57(H57), C52(H52), C8(H8), C93(H93),
 C35(H35), C60(H60), C68(H68), C61(H61), C87(H87), C66(H66), C79(H79), C81(H81),
  C78(H78), C31(H31), C7(H7), C94(H94), C82(H82), C63(H63), C74(H74), C75(H75),
 C88(H88), C58(H58), C50(H50), C48(H48), C49(H49), C26(H26), C51(H51), C67(H67),
  C36(H36), C38(H38), C56(H56)
7.d Tetrahedral OH refined with riding coordinates:
 O4(H4), O2(H2A), O4A(H4A), O2A(H2AA)
7.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
7.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O1(H1)
;
_shelx_res_checksum              85789
_shelx_hkl_checksum              97226
_shelx_fab_checksum              61873
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'