Solid-state reaction among [CoCl4]2−, [CuCl4]2− and [CuCl4(H2O)]2− ions through transmetalation and liquid-assisted grinding
Li, Haitao; Guo, Zhenwei; Liu, Tie; Xin, Lianxin; Guo, Fang; CrystEngComm 26 (2024) 381–387; doi:10.1039/D3CE01038D

data_7247846
_publ_section_title
;
 Solid-state reaction among [CoCl4]2&#x2212;, [CuCl4]2&#x2212; and
 [CuCl4(H2O)]2&#x2212; ions through transmetalation and liquid-assisted
 grinding
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              381
_journal_page_last               387
_journal_paper_doi               10.1039/D3CE01038D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(Cl4 Co), C14 H22 N4, 2(H2 O)'
_chemical_formula_sum            'C14 H26 Cl8 Co2 N4 O2'
_chemical_formula_weight         683.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-17 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8956(5)
_cell_length_b                   14.3091(8)
_cell_length_c                   10.4218(6)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    298.27
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.42
_cell_volume                     1325.02(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.27
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23877
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.420
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.6228.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       Block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0261P)^2^+0.5482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2868
_reflns_number_total             3256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01038d2.cif
_cod_data_source_block           mo_180508_lhd8_0m
_cod_depositor_comments
'Adding full bibliography for 7247846--7247849.cif.'
_cod_database_code               7247846
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.575
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All H(H,H) groups
2. Restrained distances
 H1AB-H1AA
 1.39 with sigma of 0.01
 O1-H1AB
 0.89 with sigma of 0.01
 O1-H1AA
 0.89 with sigma of 0.01
 H1BD-H1BC
 1.39 with sigma of 0.01
 O1-H1AA \\sim O1-H1BC
 with sigma of 0.02
 O1-H1AB \\sim O1-H1BD
 with sigma of 0.02
3. Others
 Sof(H1BC)=Sof(H1BD)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C7(H7A,H7B), C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C3(H3), C2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'