Chiral discrimination in solid-state interactions of cobalt(iii)‒polyamine complex cations with tris-(dipicolinato)lanthanate(iii) anions
Harrowfield, Jack M.; Kim, Yang; Skelton, Brian W.; Sobolev, Alexandre N.; White, Allan H.; CrystEngComm 19 (2017) 2372–; doi:10.1039/C6CE02573K

data_7228008
_publ_section_title
;
 Chiral discrimination in solid-state interactions of
 cobalt(iii)--polyamine complex cations with
 tris-(dipicolinato)lanthanate(iii) anions
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2372
_journal_paper_doi               10.1039/C6CE02573K
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C14 H30 Co N8 O4, C21 H9 Gd N3 O12, 12(H2 O)'
_chemical_formula_sum            'C35 H63 Co Gd N11 O28'
_chemical_formula_weight         1302.14
_chemical_name_common            '[Gd(dipic)3] [Co(sar)(NO2)2] * 12(H2O)'
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-15 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.6445(6)
_cell_length_b                   10.6445(6)
_cell_length_c                   36.732(3)
_cell_measurement_reflns_used    3854
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.4
_cell_volume                     3604.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL, v. 5.1'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            35559
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.301
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker area detector absorption corrections'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       prism
_exptl_crystal_F_000             1995
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 1459 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6286
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0240P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                4437
_reflns_number_total             6286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02573k2.cif
_cod_data_source_block           dgdco
_cod_depositor_comments
'Adding full bibliography for 7228006--7228011.cif.'
_cod_original_cell_volume        3604.3(5)
_cod_database_code               7228008
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              4529