Metal-Directed Synthesis of Complexes Featuring Functional P,C-Cage Ligands: What Are the Intermediates?
Streubel, Rainer; Bode, Maren; von Frantzius, Gerd; Hrib, Cristian; Jones, Peter G.; Monsees, Axel; Organometallics 26 (2007) 1371–; doi:10.1021/om0608455

data_4072581
_publ_section_title
;
 Metal-Directed Synthesis of Complexes Featuring Functional P,C-Cage
 Ligands: What Are the Intermediates?
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1371
_journal_paper_doi               10.1021/om0608455
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C30 H36 Mo O7 P2'
_chemical_formula_weight         666.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                77.195(4)
_cell_angle_beta                 83.751(4)
_cell_angle_gamma                76.866(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4632(11)
_cell_length_b                   11.4976(11)
_cell_length_c                   13.7306(12)
_cell_measurement_reflns_used    5968
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1565.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- and \f-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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27972
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    'methyls rigid and others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         9106
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                6113
_reflns_number_total             9106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608455si20060915_102238.cif
_cod_data_source_block           lilie
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4072581