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_7228007
_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, 6.5(H2 O)'
_chemical_formula_sum            'C27 H46 Co Gd N9 O18.5'
_chemical_formula_weight         1008.90
_chemical_name_common            '2[Gd(dipic)3] 2[CoEn3] * 13(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                 95.879(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4992(4)
_cell_length_b                   21.4101(9)
_cell_length_c                   16.8664(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.5
_cell_measurement_theta_min      2.5
_cell_volume                     3771.4(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 0.978
_diffrn_measured_fraction_theta_max 0.926
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77371
_diffrn_reflns_point_group_measured_fraction_full 0.501
_diffrn_reflns_point_group_measured_fraction_max 0.472
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         37.586
_diffrn_reflns_theta_min         1.542
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker area detector absorption corrections'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.604
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         18851
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                17442
_reflns_number_total             18851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02573k2.cif
_cod_data_source_block           777295
_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), 13(H2 O)'
_cod_original_formula_sum        'C54 H92 Co2 Gd2 N18 O37'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2017.81
_cod_database_code               7228007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.503
_shelx_estimated_absorpt_t_max   0.590
_shelx_res_checksum              81216