Half-sandwich complexes of molybdenum-(III), -(IV) and -(V) with P‒O and P‒N bifunctional ligands Ph2PCH2X (X = 2-oxazolinyl, or C(O)NPh2)
Camus, Jean-Michel; Morales, Dolores; Andrieu, Jacques; Richard, Philippe; Poli, Rinaldo; Braunstein, Pierre; Naud, Frédéric; Journal of the Chemical Society, Dalton Transactions  (2000) 2577–; doi:10.1039/b002403l

data_7009630
_publ_section_title
;
 Half-sandwich complexes of molybdenum-(III), -(IV) and -(V) with P--O
 and P--N bifunctional ligands Ph2PCH2X
 (X&#x2005;=&#x2005;2-oxazolinyl, or C(O)NPh2)
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2577
_journal_paper_doi               10.1039/b002403l
_journal_year                    2000
_chemical_formula_moiety         'C36 H37 Cl3 Mo N O P, B F4'
_chemical_formula_sum            'C36 H37 B Cl3 F4 Mo N O P'
_chemical_formula_weight         819.74
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.961(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3540(10)
_cell_length_b                   14.8950(10)
_cell_length_c                   19.9370(10)
_cell_measurement_reflns_used    27933
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3509.1(4)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       collect
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997) '
_diffrn_ambient_temperature      110(2)
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24328
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.984
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+12.9265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1537
_refine_ls_wR_factor_gt          0.1368
_reflns_number_gt                5910
_reflns_number_total             8008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002403l.txt
_cod_data_source_block           p21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+12.9265P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+12.9265P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7009630