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_7248045
_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
_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            4
_cell_length_a                   9.5688(2)
_cell_length_b                   12.9473(3)
_cell_length_c                   15.9128(3)
_cell_measurement_reflns_used    15918
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.461
_cell_measurement_theta_min      4.402
_cell_volume                     1971.44(7)
_computing_cell_refinement       SAINT
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        SAINT
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15918
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.461
_diffrn_reflns_theta_min         4.402
_exptl_absorpt_coefficient_mu    11.888
_exptl_absorpt_correction_T_max  0.383
_exptl_absorpt_correction_T_min  0.269
_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    1.540
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3757
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0296P)^2^+0.5444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                3279
_reflns_number_total             3757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00759f2.cif
_cod_data_source_block           COMPOUND_C_RT
_cod_database_code               7248045
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.269
_exptl_absorpt_special_details   prismatic
_olex2_refinement_description
;
1. 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
2. Restrained distances
 H2AB-Cl4_$1
 2.06 with sigma of 0.02
 O2A-H2AB
 0.84 with sigma of 0.02
 N2-C12 \\sim N2A-C12A
 with sigma of 0.02
 N2-C13 \\sim N2A-C13A
 with sigma of 0.02
 N2-C14 \\sim N2A-C14A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C8-C10 \\sim C8A-C10A
 with sigma of 0.02
 C8-C11 \\sim C8A-C11A
 with sigma of 0.02
 C9-C12 \\sim C9A-C12A
 with sigma of 0.02
 C10-C13 \\sim C10A-C13A
 with sigma of 0.02
 C11-C14 \\sim C11A-C14A
 with sigma of 0.02
 C11-O2 \\sim C11A-O2A
 with sigma of 0.02
 N2-C9 \\sim N2A-C9A
 with sigma of 0.04
 N2-C10 \\sim N2A-C10A
 with sigma of 0.04
 N2-C11 \\sim N2A-C11A
 with sigma of 0.04
 C8-C12 \\sim C8A-C12A
 with sigma of 0.04
 C8-C13 \\sim C8A-C13A
 with sigma of 0.04
 C8-C14 \\sim C8A-C14A
 with sigma of 0.04
 C8-O2 \\sim C8A-O2A
 with sigma of 0.04
 C9-C10 \\sim C9A-C10A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C10-C11 \\sim C10A-C11A
 with sigma of 0.04
 C12-C13 \\sim C12A-C13A
 with sigma of 0.04
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
 C13-C14 \\sim C13A-C14A
 with sigma of 0.04
 C14-O2 \\sim C14A-O2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O2A)
Uanis(C11A) = Uanis(C11)
Uanis(C8A) = Uanis(C8)
Uanis(C9) = Uanis(C9A)
Uanis(C12) = Uanis(C12A)
Uanis(C14A) = Uanis(C14)
Uanis(N2A) = Uanis(N2)
Uanis(C10) = Uanis(C10A)
Uanis(C13) = Uanis(C13A)
4. Rigid body (RIGU) restrains
 C11, C8, C14, C9, C10, N2, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N2A)=Sof(H2AA)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11A)=Sof(C8A)=Sof(H8A)=Sof(O2A)=Sof(H2AB)=1-
 FVAR(1)
 Sof(N2)=Sof(H2)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(O2)=Sof(H2A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(HA), N2(H2), C1(HB), C4(HG), C8(H8), C11(H11), N2A(H2AA), C11A(H11A),
 C8A(H8A)
6.b Secondary CH2 refined with riding coordinates:
 C2(HC,HD), C3(HE,HF), C5(HH,HI), C6(HJ,HK), C7(HL,HM), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C12A(H12C,H12D),
 C13A(H13C,H13D), C14A(H14C,H14D), C9A(H9AA,H9AB), C10A(H10C,H10D)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H), O2(H2A), O2A(H2AB)
;
_shelx_res_checksum              98260
_olex2_submission_special_instructions 'No special instructions were received'