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_7021720
_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         'C52 H52 Cl4 O2 P2 Ru2, C H2 Cl2'
_chemical_formula_sum            'C53 H54 Cl6 O2 P2 Ru2'
_chemical_formula_weight         1199.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.437(4)
_cell_angle_beta                 91.368(4)
_cell_angle_gamma                92.086(4)
_cell_formula_units_Z            2
_cell_length_a                   11.277(4)
_cell_length_b                   12.280(4)
_cell_length_c                   21.270(7)
_cell_measurement_reflns_used    2554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.41
_cell_volume                     2929.2(17)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43808
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.6236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008b)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Slab
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Following several attempts to model the disorder in a site
partially occupied by solvent dichloromethane which proved unsuccessful,
the density in this site was removed with the SQUEEZE option of PLATON
(SPEK, 2010).
;
_refine_diff_density_max         1.603
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         12820
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0773P)^2^+7.1225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                10168
_reflns_number_total             12820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51046h.txt
_cod_data_source_block           msb488_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               7021720