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_4082670
_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         'C8 H16 N, C48 H40 B Mo N2 O3 P2, C4 H8 O'
_chemical_formula_sum            'C60 H64 B Mo N3 O4 P2'
_chemical_formula_weight         1059.83
_chemical_name_common            13169a
_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                 106.177(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7468(13)
_cell_length_b                   19.4959(18)
_cell_length_c                   20.5752(19)
_cell_measurement_reflns_used    2979
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.31
_cell_volume                     5295.9(9)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            54985
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.8640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+5.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                6665
_reflns_number_total             10051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5001056_si_003.cif
_cod_data_source_block           13169a
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082670