Structural and Spectroscopic Investigations of Two [Cu<sub>4</sub>X<sub>6</sub>]<sup>2-</sup> (X = Cl<sup>-</sup>, Br<sup>-</sup>) Clusters: A Joint Theoretical and Experimental Work.
Latouche, Camille; Gautier, Romain; Génois, Romain; Massuyeau, Florian; The journal of physical chemistry. A 122 (2018) 4628–4634; doi:10.1021/acs.jpca.8b02663

data_1552784
_publ_section_title
;
 Structural and Spectroscopic Investigations of Two
 [Cu<sub>4</sub>X<sub>6</sub>]<sup>2-</sup> (X = Cl<sup>-</sup>,
 Br<sup>-</sup>) Clusters: A Joint Theoretical and Experimental Work.
;
_journal_issue                   19
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              4628
_journal_page_last               4634
_journal_paper_doi               10.1021/acs.jpca.8b02663
_journal_volume                  122
_journal_year                    2018
_chemical_formula_moiety         'Cl12 Cu6, 3(C6 H16 N2), O'
_chemical_formula_sum            'C18 H50 Cl12 Cu6 N6 O'
_chemical_formula_weight         1173.28
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3441(13)
_cell_length_b                   14.6101(9)
_cell_length_c                   20.1415(19)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3926.8(6)
_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    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker-Nonius Kappa CCD diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31711
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.794
_diffrn_reflns_theta_min         6.421
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    4.031
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0847 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.8283.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 1545 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.471(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+5.0164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                4721
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b02663_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               1552784
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1C,H1D)
2.b Ternary CH refined with riding coordinates:
 N11(H11), N20(H20), N4(H4), N5(H5), N2(H2), N3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C21(H21A,H21B), C0AA(H0AA,H0AB), C6(H6A,H6B),
 C7(H7A,H7B), C10(H10A,H10B), C18(H18A,H18B), C1(H1A,H1B), C8(H8A,H8B), C9(H9A,
 H9B), C12(H12A,H12B)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C24(H24A,H24B,
 H24C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'