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_7244385
_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         'C40 H34 Co3 Gd N3 O25'
_chemical_formula_sum            'C40 H34 Co3 Gd N3 O25'
_chemical_formula_weight         1290.74
_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             2021-08-24
_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                86.370(8)
_cell_angle_beta                 84.284(8)
_cell_angle_gamma                65.297(8)
_cell_formula_units_Z            2
_cell_length_a                   10.1882(12)
_cell_length_b                   10.2651(13)
_cell_length_c                   23.231(3)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.30
_cell_measurement_theta_min      3.83
_cell_volume                     2195.6(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.967
_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  0.1270
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76045
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         1.912
_exptl_absorpt_coefficient_mu    19.214
_exptl_absorpt_correction_T_max  0.7539
_exptl_absorpt_correction_T_min  0.4498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1489 before and 0.0850 after correction.
The Ratio of minimum to maximum transmission is 0.5966.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.869
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00060(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         7796
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0847P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5722
_reflns_number_total             7796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08797e2.cif
_cod_data_source_block           tnd525a5
_cod_original_cell_volume        2195.7(5)
_cod_database_code               7244385
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.174
_shelx_estimated_absorpt_t_min   0.139
_olex2_refinement_description
;
1. 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
2. Restrained distances
 O14-H14
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 O15-H15
 0.87 with sigma of 0.01
 O16-H16
 0.87 with sigma of 0.01
 C62-H15
 1.931098 with sigma of 0.02
 C60-H13
 1.935026 with sigma of 0.02
 C63-H16
 1.87848 with sigma of 0.02
 Co2-H13
 2.638926 with sigma of 0.02
 Co3-H15
 2.641059 with sigma of 0.02
 C61-H14
 1.915442 with sigma of 0.02
 Co3-H16
 2.644399 with sigma of 0.02
 Co2-H14
 2.657869 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C26(H26), C46(H46), C29(H29), C11(H11), C47(H47), C49(H49),
 C31(H31), C51(H51), C12(H12), C27(H27), C48(H48), C9(H9), C32(H32), C6(H6),
 C28(H28), C7(H7), C8(H8)
3.b Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              95829
_olex2_submission_special_instructions 'No special instructions were received'