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_4305266
_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_sum            'C36 H81 Cl O3 Si3 W'
_chemical_formula_weight         865.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.993(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4736(1)
_cell_length_b                   23.0999(3)
_cell_length_c                   11.5577(1)
_cell_measurement_temperature    173(2)
_cell_volume                     2220.78(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_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      173(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       '0.3 deg. \w-scan'
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10249
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.611670
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.127
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5629
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_obs          0.0345
_refine_ls_shift/esd_max         1.000
_refine_ls_shift/esd_mean        0.155
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+6.1390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0903
_refine_ls_wR_factor_obs         0.0786
_reflns_number_observed          5259
_reflns_number_total             6859
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic800139c-file001_3.cif
_cod_data_source_block           ro3w
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+6.1390P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+6.1390P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4305266