Synthesis of Tungsten and Molybdenum Carbon Dioxide Complexes
Carden, Robert G.; Ohane, James J.; Pike, Robert D.; Graham, Peter M.; Organometallics 32 (2013) 2505–; doi:10.1021/om4002022

data_4080807
_publ_section_title
;
 Synthesis of Tungsten and Molybdenum Carbon Dioxide Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2505
_journal_paper_doi               10.1021/om4002022
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C13 H19 B N7 O3 P W'
_chemical_formula_sum            'C13 H19 B N7 O3 P W'
_chemical_formula_weight         546.98
_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                 104.0900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3695(3)
_cell_length_b                   12.4462(3)
_cell_length_c                   14.5269(4)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      3.14
_cell_volume                     1818.45(9)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXLE (Hubschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD'
_diffrn_measurement_method       '\w and \y'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18789
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.874
_exptl_absorpt_correction_T_max  0.4492
_exptl_absorpt_correction_T_min  0.1253
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.094
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.606
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3173
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.603
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                3010
_reflns_number_total             3173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002022_si_002.cif
_cod_data_source_block           p21onn
_cod_original_cell_volume        1818.45(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4080807