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_7244387
_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         'C36 H30 Co3 La N2 O24, H2 O, N O3'
_chemical_formula_sum            'C42 H47 Co3 La N3 O29.5'
_chemical_formula_weight         1381.52
_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                93.324(7)
_cell_angle_beta                 108.261(8)
_cell_angle_gamma                90.444(6)
_cell_formula_units_Z            2
_cell_length_a                   10.2888(8)
_cell_length_b                   15.4555(13)
_cell_length_c                   16.0338(14)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    102.0
_cell_measurement_theta_max      73.20
_cell_measurement_theta_min      2.86
_cell_volume                     2416.3(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      102.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_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  0.1021
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34920
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.865
_exptl_absorpt_coefficient_mu    15.544
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.4962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.6581.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.00234(19)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0804
_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^)+(0.0982P)^2^+27.2887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5934
_reflns_number_total             8664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08797e2.cif
_cod_data_source_block           tnd525a8
_cod_original_formula_sum        'C42 H47 Co3 La N3 O29.50'
_cod_database_code               7244387
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.220
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N30B-O31B \\sim N30B-O32B \\sim N30B-O33B
 with sigma of 0.02
 O31B-O32B \\sim O32B-O33B \\sim O33B-O31B
 with sigma of 0.04
3. Restrained planarity
 N30B, O31B, O32B, O33B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N30B \\sim O31B \\sim O32B \\sim O33B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N30B) \\sim Ueq, Uanis(O31B) \\sim Ueq, Uanis(O32B) \\sim Ueq,
Uanis(O33B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N30A) \\sim Ueq, Uanis(O31A) \\sim Ueq, Uanis(O32A) \\sim Ueq,
Uanis(O33A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N30B, O31B, O32B, O33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N30A)=Sof(O31A)=Sof(O32A)=Sof(O33A)=1-FVAR(1)
 Sof(N30B)=Sof(O31B)=Sof(O32B)=Sof(O33B)=FVAR(1)
7.a Free rotating group:
 O25(H25A,H25B), N30B(O31B,O32B,O33B)
7.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,
 H18B), O17(H17A,H17B)
7.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C52(H52), C9(H9), C31(H31), C10(H10), C46(H46), C11(H11),
 C27(H27), C6(H6), C47(H47), C29(H29), C49(H49), C48(H48), C51(H51), C32(H32),
 C28(H28), C26(H26)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16645
_shelx_fab_checksum              1518
_olex2_submission_special_instructions 'No special instructions were received'