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_7245180
_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         '3(Cl4 Cu), 2(C19 H19 N4)'
_chemical_formula_sum            'C38 H38 Cl12 Cu3 N8'
_chemical_formula_weight         1222.78
_chemical_melting_point          397.4(7)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 96.956(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8177(4)
_cell_length_b                   25.0982(14)
_cell_length_c                   12.3248(7)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.322
_cell_measurement_theta_min      2.950
_cell_volume                     2400.5(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31301
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.933
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       plate
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.110(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8386
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0395
_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^)+(0.0243P)^2^+2.3017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7740
_reflns_number_total             8386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00624c2.cif
_cod_data_source_block           20191225_gf_zhj_2a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '396.75-398.05' was changed
to '397.4(7)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7245180
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.890(15)
 0.110(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C33(H33A,H33B), C6(H6A,H6B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N5(H5), N4(H4), N1(H1), C26(H26), C16(H16), C7(H7), C19(H19),
 C23(H23), C35(H35), C28(H28), C29(H29), C20(H20), C36(H36), C31(H31), C18(H18),
  C9(H9), C2(H2), C38(H38), C30(H30), C21(H21), C22(H22), C4(H4A), C37(H37),
 C10(H10), C3(H3), C17(H17), C1(H1A), C12(H12), C11(H11)
;
_shelx_res_checksum              96729
_shelx_hkl_checksum              1177
_olex2_submission_special_instructions 'No special instructions were received'