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_7247848
_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         'Cl4 Cu, 2(Cl), C14 H22 N4'
_chemical_formula_sum            'C14 H22 Cl6 Cu N4'
_chemical_formula_weight         522.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-19
_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                 93.543(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1035(8)
_cell_length_b                   5.0596(4)
_cell_length_c                   23.3576(19)
_cell_measurement_reflns_used    4761
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      2.76
_cell_volume                     1073.80(15)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      293.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9534
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.756
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.7587.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+2.5157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1640
_reflns_number_total             1882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01038d2.cif
_cod_data_source_block           230919_l1_0m_a
_cod_depositor_comments
'Adding full bibliography for 7247846--7247849.cif.'
_cod_database_code               7247848
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.719
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Others
 Sof(Cu1A)=0.5*(1-FVAR(2))
 Sof(Cu1)=0.5*FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C4(H4), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'