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_7234649
_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         'Cl8 Cu2, H2 O, C18 H28 N4'
_chemical_formula_sum            'C18 H30 Cl8 Cu2 N4 O'
_chemical_formula_weight         729.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-30 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6563(5)
_cell_length_b                   11.4146(7)
_cell_length_c                   24.6751(14)
_cell_measurement_reflns_used    9314
_cell_measurement_temperature    173.01
_cell_measurement_theta_max      28.311
_cell_measurement_theta_min      3.053
_cell_volume                     2719.8(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.01
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36360
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.884
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1099 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.6189.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.518
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 1956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0292P)^2^+1.1085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                4663
_reflns_number_total             4700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00911f2.cif
_cod_data_source_block           20180523_4b_0m
_cod_database_code               7234649
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.589
_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 Free rotating group:
 O1(H,HA)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C12(H12)
2.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C6(H6A,
 H6B), C11(H11A,H11B), C13(H13A,H13B)
2.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C4(H4A), C2(H2), C15(H15), C18(H18), C1(H1A), C17(H17),
 C14(H14), C5(H5)
;
_shelx_res_checksum              33979
_olex2_submission_special_instructions 'No special instructions were received'