New bisphosphomide ligands, 1,3-phenylenebis((diphenylphosphino)methanone) and (2-bromo-1,3-phenylene)bis((diphenylphosphino)methanone): synthesis, coordination behavior, DFT calculations and catalytic studies.
Kumar, Pawan; Siddiqui, Mujahuddin M.; Reddi, Yerrnaidu; Mague, Joel T.; Sunoj, Raghavan B.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11385–11399; doi:10.1039/c3dt51046h

data_7021725
_publ_section_title
;
 New bisphosphomide ligands,
 1,3-phenylenebis((diphenylphosphino)methanone) and
 (2-bromo-1,3-phenylene)bis((diphenylphosphino)methanone): synthesis,
 coordination behavior, DFT calculations and catalytic studies.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11385
_journal_page_last               11399
_journal_paper_doi               10.1039/c3dt51046h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C64 H48 Cu2 I2 O4 P4, C4 H8 0'
_chemical_formula_sum            'C68 H56 Cu2 I2 O5 P4'
_chemical_formula_weight         1457.89
_chemical_name_systematic
;
\m-Diiodobis(\m-(3-diphenylphosphanecarbonylphenyl)-
diphenylphosphanylmethanone)dicopper(I) tetrahydrofuran
solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.317(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0999(19)
_cell_length_b                   29.083(4)
_cell_length_c                   18.143(3)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.36
_cell_volume                     6482.2(17)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54692
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.7712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         14289
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0356P)^2^+10.1897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                10308
_reflns_number_total             14289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51046h.txt
_cod_data_source_block           msb408_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6482.3(16)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7021725