Synthesis and structure of CpMo(CO)(dppe)H and its oxidation by Ph3C+.
Cheng, Tan-Yun; Szalda, David J.; Zhang, Jie; Bullock, R. Morris; Inorganic chemistry 45 (2006) 4712–4720; doi:10.1021/ic060111k

data_4350243
_publ_section_title
;
 Synthesis and structure of CpMo(CO)(dppe)H and its oxidation by Ph3C+.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4712
_journal_page_last               4720
_journal_paper_doi               10.1021/ic060111k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
; 
'(C32 H30 O1 P2  Mo1), (C7 H8)' 
;
_chemical_formula_sum            'C39 H38 Mo O P2'
_chemical_formula_weight         680.57
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                96.65(2)
_cell_angle_beta                 105.50(2)
_cell_angle_gamma                96.43(2)
_cell_formula_units_Z            2
_cell_length_a                   10.830(3)
_cell_length_b                   11.307(3)
_cell_length_c                   14.309(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1658.3(8)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4VAX (Sheldrick, 1993)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2650
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7590
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.93111
_exptl_absorpt_correction_T_min  0.91010
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
 Sheldrick, G. M., 1994, SHELXL Version 5, Siemens Analytical Instruments,
 Inc., Madison WI

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .17
_refine_diff_density_max         0.618
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.2393
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                3322
_reflns_number_total             7590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060111ksi20060119_101922.cif
_cod_data_source_block           tanyun
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'GAUSSIAN' was
changed to 'gaussian' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4350243