Reactions of [W2(OCH2tBu)8] (M?M) with diazobenzene and trimethylsilyldiazomethane. Preparation and structures of W2(OCH2tBu)8(NPh) and W2(OCH2tBu)8(N2C(H)SiMe3)
Chisholm, Malcolm H.; Click, Damon R.; Gallucci, Judith C.; Hadad, Christopher M.; Dalton Transactions  (2003) 3205–; doi:10.1039/b304587k

data_7013114
_publ_section_title
;
 Reactions of [W2(OCH2tBu)8] (M?M) with diazobenzene and
 trimethylsilyldiazomethane. Preparation and structures of
 W2(OCH2tBu)8(NPh) and W2(OCH2tBu)8(N2C(H)SiMe3)
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3205
_journal_paper_doi               10.1039/b304587k
_journal_year                    2003
_chemical_formula_moiety         '(C46 H93 N O8 W2), C3 H7'
_chemical_formula_sum            'C49 H100 N O8 W2'
_chemical_formula_weight         1199.00
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                92.84(1)
_cell_angle_beta                 99.67(1)
_cell_angle_gamma                102.96(1)
_cell_formula_units_Z            2
_cell_length_a                   12.030(1)
_cell_length_b                   12.048(1)
_cell_length_c                   20.567(2)
_cell_measurement_temperature    200(2)
_cell_volume                     2851.9(5)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and 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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63505
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.075
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       'rectangular rod'
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.006
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         13080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         -0.096
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+4.6791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0613
_refine_ls_wR_factor_obs         0.0569
_reflns_number_observed          10310
_reflns_number_total             13080
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b304587k.txt
_cod_data_source_block           Chisholm985
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+4.6791P] 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^)+(0.0121P)^2^+4.6791P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               7013114