Group VI Metal Carbonyl Complexes of Bis((diphenylphosphino)methyl)diphenylborate and an Assessment of Their Utility for Template Ligand Syntheses
Fischer, Paul J.; Avena, Laura; Bohrmann, Trent D.; Neary, Michelle C.; Putka, Grace K.; Sullivan, Kevin P.; Organometallics 33 (2014) 1300–; doi:10.1021/om5001056

data_4082658
_publ_section_title
;
 Group VI Metal Carbonyl Complexes of
 Bis((diphenylphosphino)methyl)diphenylborate and an Assessment of Their
 Utility for Template Ligand Syntheses
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1300
_journal_paper_doi               10.1021/om5001056
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C42 H34 B Cr O4 P2, C8 H16 N, C4 H8 O'
_chemical_formula_sum            'C54 H58 B Cr N O5 P2'
_chemical_formula_weight         925.76
_chemical_name_common            13227a
_chemical_name_systematic
; 
 ? 
;
_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                 91.595(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1950(11)
_cell_length_b                   21.560(2)
_cell_length_c                   19.656(2)
_cell_measurement_reflns_used    2920
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.14
_cell_measurement_theta_min      4.45
_cell_volume                     4742.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-AXS D8 Photon-100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'parallel mirrors'
_diffrn_radiation_source         'ImuS microfocus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41532
_diffrn_reflns_theta_full        68.48
_diffrn_reflns_theta_max         68.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.010
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012/1)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         8611
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0847P)^2^+4.3058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                7630
_reflns_number_total             8611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5001056_si_003.cif
_cod_data_source_block           13227a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4742.6(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082658