Mechanosynthesis of polymeric and binuclear copper complexes via dehydrochlorination and their application in solvent-free C–S bond cross-coupling
Hao, Xiujia; Li, Xinyu; Li, Haitao; Zhang, Xin; Liu, Xiaozhi; Guo, Fang; CrystEngComm  (2022) –; doi:10.1039/D2CE00624C

data_7245179
_publ_section_title
;
 Mechanosynthesis of polymeric and binuclear copper complexes via
 dehydrochlorination and their application in solvent-free C--S bond
 cross-coupling
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00624C
_journal_year                    2022
_chemical_formula_moiety         'Cl4 Cu, Cl, C15 H17 N4'
_chemical_formula_sum            'C15 H17 Cl5 Cu N4'
_chemical_formula_weight         494.11
_chemical_melting_point          365.2(13)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                104.664(7)
_cell_angle_beta                 110.573(7)
_cell_angle_gamma                110.692(8)
_cell_formula_units_Z            2
_cell_length_a                   10.502(2)
_cell_length_b                   10.560(3)
_cell_length_c                   11.248(3)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.313
_cell_measurement_theta_min      3.069
_cell_volume                     985.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17315
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         3.069
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1074 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.6833.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       needle
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0295P)^2^+0.7515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4441
_reflns_number_total             4802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00624c2.cif
_cod_data_source_block           20190408_2a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '363.95-366.55' was changed
to '365.2(13)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H34 Cl10 Cu2 N8'
_cod_original_formula_weight         988.23
_cod_original_formula_moiety         '2(Cl4 Cu), 2(Cl), 2(C15 H17 N4)'
_cod_original_formula_units_Z            1
_cod_database_code               7245179
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.827
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C1(H1), C2(H2), C12(H12), C6(H6), C13(H13), C9(H9), C7(H7), C8(H8),
 C14(H14), C15(H15)
;
_shelx_res_checksum              24918
_shelx_hkl_checksum              85371
_olex2_submission_special_instructions 'No special instructions were received'