Bis(<i>tert</i>-butylimido)[2-(dimethylaminomethyl)pyrrol-1-yl]tungsten(VI)-μ-oxo-bis(<i>tert</i>-butylimido)(η^2^-<i>N,O</i>-<i>tert</i>-butylnitroso)tungsten(VI)
Uno, Chia-Liang; Kuo, Pei-Cheng; Lee, Hon Man; Huang, Jui-Hsien; Acta Crystallographica Section E 61 (2005) m697–m698; doi:10.1107/S1600536805007610

data_2205396
_publ_section_title
Bis(<i>tert</i>-butylimido)[2-(dimethylaminomethyl)pyrrol-1-yl]tungsten(VI)-\m-oxo-bis(<i>tert</i>-butylimido)(\h^2^-<i>N,O</i>-<i>tert</i>-butylnitroso)tungsten(VI)
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m697
_journal_page_last               m698
_journal_paper_doi               10.1107/S1600536805007610
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[W2 (C4 H9 N)4 (C7 H11 N2) (C4 H10 N O) O]'
_chemical_formula_moiety         'C27 H57 N7 O2 W2'
_chemical_formula_sum            'C27 H57 N7 O2 W2'
_chemical_formula_weight         879.50
_chemical_name_systematic
;
Bis(tert-butylimido)[2-(dimethylaminomethyl)pyrrol-1-yl]tungsten(VI)-\m-oxo-
bis(tert-butylimido)(\h^2^-N,O-tert-butylnitroso)tungsten(VI)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.334(2)
_cell_angle_beta                 79.479(2)
_cell_angle_gamma                83.175(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6263(3)
_cell_length_b                   12.0153(3)
_cell_length_c                   15.6375(4)
_cell_measurement_reflns_used    5880
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.3
_cell_volume                     1764.02(8)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25718
_diffrn_reflns_theta_full        28.87
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.547
_exptl_absorpt_correction_T_max  0.171
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.040
_refine_diff_density_min         -1.897
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0236P)^2^+3.8003P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                7668
_reflns_number_total             9142
_reflns_threshold_expression     I>2\s
_cod_data_source_file            ac6163.cif
_cod_data_source_block           I
_cod_database_code               2205396
_cod_database_fobs_code          2205396