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_7248047
_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_formula_moiety         'C7 H16 N2, Cl4 Co, H2 O'
_chemical_formula_sum            'C7 H18 Cl4 Co N2 O'
_chemical_formula_weight         346.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_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                 91.907(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4979(4)
_cell_length_b                   16.0144(10)
_cell_length_c                   12.9534(8)
_cell_measurement_reflns_used    27064
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.665
_cell_measurement_theta_min      1.003
_cell_volume                     1347.18(14)
_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      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27064
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.778
_diffrn_reflns_theta_min         1.003
_exptl_absorpt_coefficient_mu    1.044
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.035(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0103P)^2^+1.7002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                7793
_reflns_number_total             8005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00759f2.cif
_cod_data_source_block           compound_a_100k_0m_a_CCDC1
_cod_database_code               7248047
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.965(19)
 0.035(19)
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 N(H,H,H) groups, All O(H,H) groups
3. Others
 Sof(Cl1B)=Sof(Cl3B)=Sof(Cl4B)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl3)=Sof(Cl4)=FVAR(1)
 Sof(Cl5B)=Sof(Cl7B)=Sof(Cl8B)=1-FVAR(2)
 Sof(Cl5)=Sof(Cl7)=Sof(Cl8)=FVAR(2)
4.a Free rotating group:
 O1(H1C,H1D), O2(H2F,H2G)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), C4(H4), C6(H6), C11(H11), C13(H13)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2D,H2E), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B)
4.d Me refined with riding coordinates:
 N2(H2A,H2B,H2C), N4(H4A,H4B,H4C)
;
_shelx_res_checksum              8019
_olex2_submission_special_instructions 'No special instructions were received'