Homobinuclear compounds based on a chiral oxazolidine ligand: From solid state study to aqueous solution dynamics
Areas, Esther S.; Junior, Henrique C.S.; Freitas, Brunno P.; Ferreira, Glaucio B.; Guedes, Guilherme P.; Inorganica Chimica Acta 529 (2022) 120664–; doi:10.1016/j.ica.2021.120664

data_1566019
_publ_section_title
;
 Homobinuclear compounds based on a chiral oxazolidine ligand: From solid
 state study to aqueous solution dynamics
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120664
_journal_paper_doi               10.1016/j.ica.2021.120664
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C20 H32 Cl2 Co2 N4 O8, 2(Cl)'
_chemical_formula_sum            'C20 H32 Cl4 Co2 N4 O8'
_chemical_formula_weight         716.16
_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     difmap
_cell_angle_alpha                73.400(3)
_cell_angle_beta                 88.075(2)
_cell_angle_gamma                73.363(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3616(3)
_cell_length_b                   9.0186(3)
_cell_length_c                   11.5236(5)
_cell_measurement_reflns_used    7011
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.46
_cell_volume                     701.52(5)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Mercury 4.3.1 (Macrae et al., 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23676
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         2.462
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.9090.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0169P)^2^+0.3675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2381
_reflns_number_total             2906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120664.cif
_cod_data_source_block           mo_copynoh3_0m_a
_cod_database_code               1566019
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1B), C4(H4), C2(H2A), C3(H3)
;
_shelx_res_checksum              32598