Structural and physico-chemical characterization of hybrid materials based on globular quinuclidinium cation derivatives and tetrachloridocobaltate(ii) anions
Belloso-Casuso, Cantia; de Pedro, Imanol; Canadillas-Delgado, Laura; Beobide, Garikoitz; Sánchez-Andújar, Manuel; Gárcia Ben, Javier; Walker, Julian; González Izquierdo, Palmerina; Cano, Israel; Rodríguez Fernández, Jesus; Fabelo, Oscar; CrystEngComm 26 (2024) 439–451; doi:10.1039/D3CE00759F

data_7248048
_publ_section_title
;
 Structural and physico-chemical characterization of hybrid materials
 based on globular quinuclidinium cation derivatives and
 tetrachloridocobaltate(ii) anions
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              439
_journal_page_last               451
_journal_paper_doi               10.1039/D3CE00759F
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C7 H14 N O), Cl4 Co'
_chemical_formula_sum            'C14 H28 Cl4 Co N2 O2'
_chemical_formula_weight         457.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-05 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   9.5314(12)
_cell_length_b                   15.705(2)
_cell_length_c                   38.490(5)
_cell_measurement_reflns_used    50126
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      72.644
_cell_measurement_theta_min      2.296
_cell_volume                     5761.6(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'Mitegen 200um'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            50126
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.644
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'ImS 3.0 micro source'
_exptl_absorpt_coefficient_mu    12.203
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.215
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.160(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         11022
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.1011
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2876
_refine_ls_wR_factor_ref         0.3132
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                9066
_reflns_number_total             11022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00759f2.cif
_cod_data_source_block           compound_c_100k
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C42 H84 Cl12 Co3 N6 O6'
_cod_original_formula_weight         1371.34
_cod_original_formula_moiety         '6(C7 H14 N O), 3(Cl4 Co)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5761.5(12)
_cod_database_code               7248048
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.840(13)
 0.160(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 H6-O6
 0.84 with sigma of 0.02
 H6-Cl5
 2.208 with sigma of 0.02
 O4-H4
 0.84 with sigma of 0.02
 H4-Cl9
 2.254 with sigma of 0.02
 H2-Cl1
 2.259 with sigma of 0.02
 O2-H2
 0.84 with sigma of 0.02
 O1-H1
 0.84 with sigma of 0.02
 H1-Cl2_$1
 2.266 with sigma of 0.02
 H3A-Cl8
 2.342 with sigma of 0.02
 O3-H3A
 0.84 with sigma of 0.02
 O5-H5
 0.84 with sigma of 0.02
 H5-Cl9_$2
 2.303 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C40, C37, O6, C38, C36, H38, C41, H36, C39, N6, H41A, H41B, H37A, H37B, H39A,
 H39B, C42, H6C, H40A, H40B, H42A, H42B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2C), N3(H3B), N4(H4C), N5(H5C), N6(H6C), C1(H1B), C3(H3), C8(H8),
  C10(H10), C15(H15), C17(H17), C22(H22), C24(H24), C29(H29), C31(H31),
 C36(H36), C38(H38)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,
 H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3A), O4(H4), O5(H5), O6(H6)
;
_shelx_res_checksum              7672
_olex2_submission_special_instructions 'No special instructions were received'