Synthesis, Structure, and Reactivities of [η2-P7M(CO)4]3-, [η2-HP7M(CO)4]2-, and [η2-RP7M(CO)4]2-Zintl Ion Complexes Where M = Mo, W
Scott Charles; James C. Fettinger; Bryan W. Eichhorn; Inorganic Chemistry 35 (1996) 1540–1548; doi:10.1021/ic9511534

data_4323796
_publ_section_title
;
 Synthesis, Structure, and Reactivities of [\h2-P7M(CO)4]3-,
 [\h2-HP7M(CO)4]2-, and [\h2-RP7M(CO)4]2-Zintl Ion Complexes Where M = Mo,
 W
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1540
_journal_page_last               1548
_journal_paper_doi               10.1021/ic9511534
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C42 H76 K2 Mo N6 O16 P7'
_chemical_formula_weight         1312.02
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.412(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.848(2)
_cell_length_b                   12.5283(15)
_cell_length_c                   21.460(2)
_cell_measurement_temperature    153(2)
_cell_volume                     6141.0(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4125
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.595
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.135
_refine_ls_goodness_of_fit_obs   1.228
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_restrained_S_obs      1.228
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_obs          0.0681
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+28.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1610
_refine_ls_wR_factor_obs         0.1399
_reflns_number_observed          2697
_reflns_number_total             4008
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9511534_1.cif
_cod_data_source_block           159cc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+28.6848P] 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^)+(0.0597P)^2^+28.6848P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6140.9(12)
_cod_database_code               4323796