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_7245178
_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         'C19 H17 Cl3 Cu N4'
_chemical_formula_sum            'C19 H17 Cl3 Cu N4'
_chemical_formula_weight         471.26
_chemical_melting_point          413.1(6)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-07 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.858(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1471(9)
_cell_length_b                   13.7121(12)
_cell_length_c                   14.0607(12)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      28.355
_cell_measurement_theta_min      2.901
_cell_volume                     1953.9(3)
_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)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30290
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.901
_exptl_absorpt_coefficient_mu    1.540
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0322P)^2^+4.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4225
_reflns_number_total             4844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00624c2.cif
_cod_data_source_block           2020_12_08_gf_lxy_1a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '412.55-413.75' was changed
to '413.1(6)' -- 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               7245178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.813
_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:
 C8(H8A,H8B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C13(H13), C12(H12), C10(H10), C6(H6), C11(H11), C3(H3), C4(H4),
 C5(H5), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              97801
_shelx_hkl_checksum              94976
_olex2_submission_special_instructions 'No special instructions were received'