Stoichiometry mechanosynthesis and interconversion of metal salts containing [CuCl3(H2O)]- and [Cu2Cl8]4-
Guo, Fang; Li, Hai Tao; Famulari, Antonino; Xin, Lianxin; Zhou, Hongjian; Zhang, Peng; CrystEngComm  (2019) –; doi:10.1039/C9CE00911F

data_7234647
_publ_section_title
;
 Stoichiometry mechanosynthesis and interconversion of metal salts
 containing [CuCl3(H2O)]- and [Cu2Cl8]4-
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00911F
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl3 Cu H2 O, 3(Cl), C18 H28 N4'
_chemical_formula_sum            'C18 H30 Cl6 Cu N4 O'
_chemical_formula_weight         594.70
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-27 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9780(6)
_cell_length_b                   14.7620(13)
_cell_length_c                   12.3395(10)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.328
_cell_measurement_theta_min      3.139
_cell_volume                     1251.23(18)
_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 0.979
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18666
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         3.140
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       needle
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2579 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6027
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0286P)^2^+0.6235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                5750
_reflns_number_total             6027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00911f2.cif
_cod_data_source_block           20171018_1a_0m
_cod_database_code               7234647
_shelx_shelxl_version_number     2014/7
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1C,H1D)
2.b Ternary CH refined with riding coordinates:
 C6(H6), C1(H1)
2.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C5(H5A,H5B), C7(H7A,H7B), C13(H13A,H13B), C2(H2C,
 H2D), C4(H4A,H4B), C3(H3A,H3B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), N3(H3), C9(H9), N4(H4), C11(H11), C14(H14), C15(H15), C12(H12),
 C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'