Lanthanide induced variability in localised CoII geometries of four triangular L3Co3IILnIII complexes
Dais, Tyson N.; Takano, Rina; Ishida, Takayuki; Plieger, Paul G.; RSC Advances 12 (2022) 4828–4835; doi:10.1039/D1RA08797E

data_7244386
_publ_section_title
;
 Lanthanide induced variability in localised CoII geometries of four
 triangular L3Co3IILnIII complexes
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4828
_journal_page_last               4835
_journal_paper_doi               10.1039/D1RA08797E
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C39.5 H33 Cl Co3 N2 O22 Tb'
_chemical_formula_sum            'C39.5 H36 Cl Co3 N2 O23.5 Tb'
_chemical_formula_weight         1285.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0045(5)
_cell_length_b                   15.7554(5)
_cell_length_c                   41.1854(16)
_cell_measurement_reflns_used    7675
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.08
_cell_measurement_theta_min      4.24
_cell_volume                     9036.6(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            36728
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.234
_diffrn_reflns_theta_min         4.237
_exptl_absorpt_coefficient_mu    17.370
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.5196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1221 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.6891.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.070
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         8148
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5445
_reflns_number_total             8148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08797e2.cif
_cod_data_source_block           tnd525a9
_cod_original_formula_sum        'C39.50 H36 Cl Co3 N2 O23.50 Tb'
_cod_database_code               7244386
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.276
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H14 of O14
 At 1.5 times of:
  All C(H,H,H) groups, H15 of O15, H17 of O17, H16 of O16, All O(H,H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
 O17-H17
 0.87 with sigma of 0.01
 O15-H15
 0.87 with sigma of 0.01
 Co2-H15
 2.668262 with sigma of 0.02
 Co3-H17
 2.608347 with sigma of 0.02
 C63-H17
 1.93834 with sigma of 0.02
 C61-H15
 1.868255 with sigma of 0.02
 C62-H16
 1.894333 with sigma of 0.02
 Co3-H16
 2.751897 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5) O14(0.5) H14(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5)
5.a Rotating group:
 O13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C31(H31), C29(H29), C52(H52), C32(H32), C51(H51), C9(H9), C6(H6),
 C26(H26), C46(H46), C8(H8), C28(H28), C11(H11), C7(H7), C48(H48), C47(H47),
 C49(H49), C27(H27), O14(H14)
5.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C61(H61A,H61B,H61C), C60(H60A,H60B,
 H60C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75808
_shelx_fab_checksum              87295
_olex2_submission_special_instructions 'No special instructions were received'