Novel carbon dioxide and carbonyl carbonate complexes of molybdenum. The X-ray structures of trans-[Mo(CO2)2{HN(CH2CH2PMe2)2}(PMe3)] and [Mo3(µ2-CO3)(µ2-O)2(O)2(CO)2(H2O)(PMe3)6]·H2O
Leopoldo Contreras; Margarita Paneque; Murielle Sellin; Ernesto Carmona; Pedro J. Pérez; Enrique Gutiérrez-Puebla; Angeles Monge; Caridad Ruiz; New Journal of Chemistry 29 (2005) 109–; doi:10.1039/b409385b

data_7052409
_publ_section_title
;
 Novel carbon dioxide and carbonyl carbonate complexes of molybdenum.
 The X-ray structures of trans-[Mo(CO2)2{HN(CH2CH2PMe2)2}(PMe3)] and
 [Mo3(&#x00B5;2-CO3)(&#x00B5;2-O)2(O)2(CO)2(H2O)(PMe3)6]&#x00B7;H2O
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              109
_journal_paper_doi               10.1039/b409385b
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C14.5 H34 Mo N O4 P3'
_chemical_formula_weight         474.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.878(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.947(5)
_cell_length_b                   11.670(2)
_cell_length_c                   20.004(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4557(2)
_computing_cell_refinement       'NONIUS CAD4'
_computing_data_collection       'NONIUS CAD4'
_computing_data_reduction        'NONIUS CAD4'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'NONIUS CAD4'
_diffrn_measurement_method       '2O/w scans'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.1840
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5616
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.801
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.2355
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.140
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1387P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.2384
_reflns_number_gt                2281
_reflns_number_total             5459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b409385b.txt
_cod_data_source_block           mse11
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C13 H30 N O4 P3 Mo ( C3 H8 )0.5'
_cod_database_code               7052409