Tetra-μ~3~-iodido-tetrakis[(tri-<i>n</i>-butylphosphane-κ<i>P</i>)copper(I)]
Klenk, Simon; Frey, Wolfgang; Bubrin, Martina; Laschat, Sabine; Acta Crystallographica Section E 70 (2014) m117–m118; doi:10.1107/S1600536814003390

data_2239242
_publ_section_title
;
 Tetra-\m~3~-iodido-tetrakis[(tri-<i>n</i>-butylphosphane-\k<i>P</i>)copper(I)]
;
_journal_coeditor_code           HP2064
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m117
_journal_page_last               m118
_journal_paper_doi               10.1107/S1600536814003390
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cu4 I4 (C12 H27 P1)4]'
_chemical_formula_moiety         'C48 H108 Cu4 I4 P4'
_chemical_formula_sum            'C48 H108 Cu4 I4 P4'
_chemical_formula_weight         1570.98
_chemical_name_systematic
;
Tetra-\m~3~-iodido-tetrakis[(tri-<i>n</i>-butylphosphane-\k<i>P</i>)copper(I)]
;
_space_group_IT_number           158
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.006(2)
_cell_length_b                   22.006(2)
_cell_length_c                   23.276(2)
_cell_measurement_reflns_used    10102
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      1.75
_cell_volume                     9761.6(15)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89010
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.8520
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.161
_refine_ls_abs_structure_details 'Flack (1983), 6695 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         13415
_refine_ls_number_restraints     341
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+46.6098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                10102
_reflns_number_total             13415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hp2064sup1.cf
_cod_data_source_block           I
_cod_database_code               2239242
_cod_database_fobs_code          2239242