Molybdenum and Tungsten Structural Differences are Dependent on ndz2/(n+1)s Mixing: Comparisons of (silox)3MX/R (M = Mo, W; silox =tBu3SiO)
David S. Kuiper; Richard E. Douthwaite; Ana-Rita Mayol; Peter T. Wolczanski; Emil B. Lobkovsky; Thomas R. Cundari; Oanh P. Lam; Karsten Meyer; Inorganic Chemistry 47 (2008) 7139–7153; doi:10.1021/ic800139c

data_4305264
_publ_section_title
;
Molybdenum and Tungsten Structural Differences are Dependent on ndz2/(n+1)s
Mixing: Comparisons of (silox)3MX/R (M = Mo, W; silox =tBu3SiO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7139
_journal_page_last               7153
_journal_paper_doi               10.1021/ic800139c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C36 H81 Cl2 O3 Si3 W'
_chemical_formula_sum            'C36 H81 Cl2 O3 Si3 W'
_chemical_formula_weight         901.03
_chemical_name_common            1-W
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.772(3)
_cell_length_b                   25.076(6)
_cell_length_c                   43.581(11)
_cell_measurement_temperature    293(2)
_cell_volume                     9586(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens P4 diffractometer'
_diffrn_measurement_method       \w/2\q
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.1203
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5247
_diffrn_reflns_theta_full        19.99
_diffrn_reflns_theta_max         19.99
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3768
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                3668
_reflns_number_total             5216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800139c-file001_1.cif
_cod_data_source_block           redtun
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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_database_code               4305264