Synthesis and oxidation of d6 tungsten pincer complexes: a complete series of tungsten(II) hydridocarbonyl and halocarbonyl pincer complexes.
Wingard, Leah A.; White, Peter S.; Templeton, Joseph L.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11438–11448; doi:10.1039/c2dt30848g

data_7030217
_publ_section_title
;
 Synthesis and oxidation of d6 tungsten pincer complexes: a complete
 series of tungsten(II) hydridocarbonyl and halocarbonyl pincer complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11438
_journal_page_last               11448
_journal_paper_doi               10.1039/c2dt30848g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C33 H36 N O3 P2 Si2 W'
_chemical_formula_sum            'C33 H36 N O3 P2 Si2 W'
_chemical_formula_weight         796.60
_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                 97.327(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8236(8)
_cell_length_b                   18.5277(13)
_cell_length_c                   14.1186(8)
_cell_measurement_reflns_used    3016
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.62
_cell_measurement_theta_min      5.91
_cell_volume                     3327.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15353
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         69.07
_diffrn_reflns_theta_min         5.91
_exptl_absorpt_coefficient_mu    8.305
_exptl_absorpt_correction_T_max  0.6815
_exptl_absorpt_correction_T_min  0.3689
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker-AXS APEX2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.382
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00015(4)
_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   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                4566
_reflns_number_total             5881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30848g.txt
_cod_data_source_block           c08370
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7030217