Synthesis of hexanuclear molybdenum clusters containing phosphine oxide ligands
Szczepura, Lisa F.; Ooro, Betty A.; Wilson, Scott R.; Journal of the Chemical Society, Dalton Transactions  (2002) 3112–; doi:10.1039/b200792d

data_7011520
_publ_section_title
;
 Synthesis of hexanuclear molybdenum clusters containing phosphine
 oxide ligands
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3112
_journal_paper_doi               10.1039/b200792d
_journal_year                    2002
_chemical_formula_moiety         'C18 H42 Cl12 Mo6 O2 P2, 2(C H Cl3)'
_chemical_formula_sum            'C20 H44 Cl18 Mo6 O2 P2'
_chemical_formula_weight         1592.23
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.799(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0685(16)
_cell_length_b                   15.617(2)
_cell_length_c                   15.693(3)
_cell_measurement_reflns_used    923
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.6
_cell_volume                     2466.3(7)
_computing_cell_refinement       'SAINT V5 (Bruker, 1998)'
_computing_data_collection       'SMART V5 (Bruker, 1998)'
_computing_data_reduction        'SAINT V5 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL V5 (Bruker, 1998)'
_computing_publication_material  'CIFTAB (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL V5 (Bruker, 1998)'
_computing_structure_solution    'SHELXTL V5 (Bruker, 1998)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p46ka
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18342
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  552
_diffrn_standards_number         341
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  0.8692
_exptl_absorpt_correction_T_min  0.5564
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1536
_exptl_crystal_id                p46ka
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
thin glass fiber with the (0 1 -1) scattering planes roughly normal 
to the spindle axis. 
;
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     293
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3341
_reflns_number_total             4492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200792d.txt
_cod_data_source_block           p46ka
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P21/n '
_cod_database_code               7011520