A one-pot diastereoselective self assembly of C-stereogenic copper(i) diphosphine clusters.
Yang, Xiang-Yuan; Li, Yongxin; Pullarkat, Sumod A.; Inorganic chemistry 53 (2014) 10232–10239; doi:10.1021/ic501233w

data_4341116
_publ_section_title
;
 A one-pot diastereoselective self assembly of C-stereogenic copper(i)
 diphosphine clusters.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10232
_journal_page_last               10239
_journal_paper_doi               10.1021/ic501233w
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C140 H128.79 Cl16 Cu6 O15 P6'
_chemical_formula_weight         3185.47
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   constr
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_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.3752(10)
_cell_length_b                   17.3752(10)
_cell_length_c                   40.085(2)
_cell_measurement_temperature    103.(2)
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_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103.(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            45537
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4874
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.992
_refine_ls_abs_structure_details
;
Flack x determined using 3724 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.038(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         14843
_refine_ls_number_restraints     687
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1211P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.2106
_reflns_number_gt                9863
_reflns_number_total             14843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501233w_si_006.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4341116--4341121.cif.'
_cod_original_cell_volume        10480.3(14)
_cod_database_code               4341116
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