Synthesis and Crystal Structures of Two Isomerically Pure Organotransition-Metal [60]Fullerene Derivatives Containing dppb Ligands: mer-M(CO)3(dppb)(η2-C60) (M = Mo, W)
Song, Li-Cheng; Liu, Jin-Ting; Hu, Qing-Mei; Weng, Lin-Hong; Organometallics 19 (2000) 1643–; doi:10.1021/om990975w

data_4077716
_publ_section_title
;
 Synthesis and Crystal Structures of Two Isomerically Pure
 Organotransition-Metal [60]Fullerene Derivatives Containing dppb
 Ligands:&#x00A0;mer-M(CO)3(dppb)(\h2-C60) (M = Mo, W)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1643
_journal_paper_doi               10.1021/om990975w
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C105 H48 Mo O6 P2'
_chemical_formula_weight         1563.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                116.141(2)
_cell_angle_beta                 98.869(2)
_cell_angle_gamma                99.836(3)
_cell_formula_units_Z            2
_cell_length_a                   15.1176(19)
_cell_length_b                   16.2145(19)
_cell_length_c                   16.543(2)
_cell_measurement_temperature    298(2)
_cell_volume                     3464.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14484
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.303
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         12171
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.395
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                8717
_reflns_number_total             12171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990975w.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        3463.9(7)
_cod_database_code               4077716