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_7153063
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                   32.822(3)
_cell_length_b                   32.088(2)
_cell_length_c                   21.1255(9)
_cell_measurement_reflns_used    8117
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8400
_cell_measurement_theta_min      2.9601
_cell_volume                     22249(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            150166
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.966
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'Wed Nov 07 09:36:43 2012' 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             8928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
; 
 Flack x determined using 5935 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         20347
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17129
_reflns_number_total             20347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51196k.txt
_cod_data_source_block           Complex-1b_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               7153063
_shelxl_version_number           2013-3
_shelx_res_checksum              57937