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_4080806
_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         'C14 H16 B Mo N9 O3, C4 H8 O'
_chemical_formula_sum            'C18 H24 B Mo N9 O4'
_chemical_formula_weight         537.21
_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                79.7840(10)
_cell_angle_beta                 70.9250(10)
_cell_angle_gamma                73.7310(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4416(2)
_cell_length_b                   10.3470(2)
_cell_length_c                   12.6884(2)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.84
_cell_measurement_theta_min      3.70
_cell_volume                     1119.54(4)
_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  'XSHELL (Bruker, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18597
_diffrn_reflns_theta_full        66.98
_diffrn_reflns_theta_max         66.98
_diffrn_reflns_theta_min         3.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.189
_exptl_absorpt_correction_T_max  0.4519
_exptl_absorpt_correction_T_min  0.2729
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0342P)^2^+1.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3821
_reflns_number_total             3873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002022_si_002.cif
_cod_data_source_block           p1bar
_cod_original_cell_volume        1119.55(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080806