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_7244384
_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         'C41 H40 Co3 Dy N2 O24, N O3'
_chemical_formula_sum            'C41 H40 Co3 Dy N3 O27'
_chemical_formula_weight         1346.05
_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             2021-08-25
_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                91.217(7)
_cell_angle_beta                 91.740(6)
_cell_angle_gamma                116.345(6)
_cell_formula_units_Z            2
_cell_length_a                   10.2212(8)
_cell_length_b                   11.0914(10)
_cell_length_c                   22.1617(19)
_cell_measurement_reflns_used    4818
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      3.99
_cell_volume                     2248.7(4)
_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 0.976
_diffrn_measured_fraction_theta_max 0.974
_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  0.1035
_diffrn_reflns_av_unetI/netI     0.1359
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22277
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    18.174
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1125 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.6887.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.0023(2)
_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   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         8044
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1066P)^2^+21.7445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2074
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5021
_reflns_number_total             8044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08797e2.cif
_cod_data_source_block           tnd525a2
_cod_original_cell_volume        2248.7(3)
_cod_database_code               7244384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.185
_shelx_estimated_absorpt_t_min   0.138
_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, All O(H,H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
 O24-H24
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 O20-H20
 0.87 with sigma of 0.01
 Dy1-H24
 2.780927 with sigma of 0.02
 Co2-H13
 2.749258 with sigma of 0.02
 Co2-H14
 2.837201 with sigma of 0.02
 Co4-H20
 2.81928 with sigma of 0.02
 C61-H14
 1.943423 with sigma of 0.02
 C60-H13
 1.916542 with sigma of 0.02
 C62-H16
 1.894298 with sigma of 0.02
 C63-H20
 1.95254 with sigma of 0.02
 Co3-H16
 2.747829 with sigma of 0.02
 C64-H24
 1.936981 with sigma of 0.02
3.a Rotating group:
 O15(H15a,H15b)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C52(H52), C46(H46), C6(H6), C29(H29), C8(H8), C9(H9),
 C51(H51), C32(H32), C26(H26), C27(H27), C28(H28), C12(H12), C47(H47), C48(H48),
  C31(H31), C49(H49)
3.c Idealised Me refined as rotating group:
 C61(H61a,H61b,H61c), C64(H64a,H64b,H64c), C60(H60a,H60b,H60c), C62(H62a,H62b,
 H62c), C63(H63a,H63b,H63c)
;
_shelx_res_checksum              75684
_olex2_submission_special_instructions 'No special instructions were received'