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_7228006
_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         'C21 H9 Gd N3 O12, C6 H24 Co N6, 8.5(H2 O)'
_chemical_formula_sum            'C27 H50 Co Gd N9 O20.5'
_chemical_formula_weight         1044.93
_chemical_name_common            '2[Gd(dipic)3] 2[CoEn3] * 17(H2O)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                 90.391(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5112(5)
_cell_length_b                   16.4981(7)
_cell_length_c                   22.863(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.4
_cell_measurement_theta_min      2.5
_cell_volume                     3964.7(3)
_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 0.939
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            81752
_diffrn_reflns_point_group_measured_fraction_full 0.518
_diffrn_reflns_point_group_measured_fraction_max 0.482
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.609
_diffrn_reflns_theta_min         1.522
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker area detector absorption corrections'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.659
_refine_diff_density_min         -3.033
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         20280
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+5.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                15106
_reflns_number_total             20280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02573k2.cif
_cod_data_source_block           dcogdx
_cod_depositor_comments
;
Adding full bibliography for 7228006--7228011.cif.

2017-11-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
'2(C21 H9 Gd N3 O12), 2(C6 H24 Co N6), 17(H2 O)'
_cod_original_formula_sum        'C54 H100 Co2 Gd2 N18 O41'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2089.87
_cod_database_code               7228006
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.671
_shelx_estimated_absorpt_t_max   0.737
_shelx_res_checksum              15397