Synthesis of Ph2PC⋮C(CH2)5C⋮CPPh2Ligand and Its Complexation with Tungsten Carbonyls to Form a Dinuclear Paddle-Wheel and a Tetranuclear Tripodal Compound
Shiue, Tsun-Wei; Yeh, Wen-Yann; Lee, Gene-Hsiang; Peng, Shie-Ming; Organometallics 25 (2006) 4150–; doi:10.1021/om0603722

data_4075563
_publ_section_title
;
 Synthesis of Ph2PC&#x22EE;C(CH2)5C&#x22EE;CPPh2Ligand and Its
 Complexation with Tungsten Carbonyls to Form a Dinuclear Paddle-Wheel and
 a Tetranuclear Tripodal Compound
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4150
_journal_paper_doi               10.1021/om0603722
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C37 H30 O4 P2 W'
_chemical_formula_weight         784.40
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.810(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3289(6)
_cell_length_b                   13.7759(8)
_cell_length_c                   22.9406(13)
_cell_measurement_reflns_used    6841
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.35
_cell_volume                     3183.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega 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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41104
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.769
_exptl_absorpt_correction_T_max  0.3140
_exptl_absorpt_correction_T_min  0.2544
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0176P)^2^+4.6992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0506
_reflns_number_gt                7035
_reflns_number_total             7315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0603722si20060501_043122.cif
_cod_data_source_block           ic11139
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075563