A thiocyanato-bridged copper(i) cubane complex and its application in palladium-catalyzed Sonogashira coupling of aryl halides.
Trivedi, Manoj; Singh, Gurmeet; Kumar, Abhinav; Rath, Nigam P.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12849–12852; doi:10.1039/c3dt51196k

data_7153062
_publ_section_title
;
 A thiocyanato-bridged copper(i) cubane complex and its application in
 palladium-catalyzed Sonogashira coupling of aryl halides.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12849
_journal_page_last               12852
_journal_paper_doi               10.1039/c3dt51196k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C56 H88 Cu4 Fe2 N4 P4 S4'
_chemical_formula_sum            'C56 H88 Cu4 Fe2 N4 P4 S4'
_chemical_formula_weight         1435.28
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A b a 2'
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.8531(4)
_cell_length_b                   32.0553(6)
_cell_length_c                   21.0880(3)
_cell_measurement_reflns_used    7434
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5154
_cell_measurement_theta_min      3.0232
_cell_volume                     22208.1(6)
_computing_cell_refinement       'X-calibur S SAINT'
_computing_data_collection       'X-calibur S oxford'
_computing_data_reduction        'X-calibur S SAINT'
_computing_molecular_graphics    'Oxford SHELXTL'
_computing_publication_material  'Oxford SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77920
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  0.7111
_exptl_absorpt_correction_T_min  0.5971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       Needle
_exptl_crystal_F_000             8928
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 5557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         19194
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+14.4095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                14411
_reflns_number_total             19194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51196k.txt
_cod_data_source_block           Complex-1a_sq_s
_cod_depositor_comments
;
   The original value of the _space_group_name_Hall data value in the
   original file was 'A 2 -2ac'. This contradicts the value given by
   authors in _symmetry_space_group_name_Hall, and the value computed
   by http://cci.lbl.gov/cctbx/explore_symmetry.html. Therefore, the
   value of _space_group_name_Hall was changed to 'A 2 -2ab'. The
   original value is retained in the _cod_original_sg_symbol_Hall data
   item.

   Saulius Gra\<zulis
   2013-08-28
;
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7153062
_shelx_estimated_absorpt_t_min   0.597
_shelx_estimated_absorpt_t_max   0.711
_shelxl_version_number           2013-3
_shelx_res_checksum              14013