(<i>C</i>)-(2,4-Di-<i>tert</i>-butyl-6-{[(2<i>S</i>)-3,3-dimethyl-1-oxido-2-butyl]iminomethyl}phenolato)ethanol-<i>cis</i>-dioxomolybdenum(VI) at 100 K
Hartung, Jens; Greb, Marco; Svoboda, Ingrid; Fuess, Hartmut; Acta Crystallographica Section E 62 (2006) m275–m277; doi:10.1107/S1600536806000146

data_2208078
_publ_section_title
;(<i>C</i>)-(2,4-Di-<i>tert</i>-butyl-6-{[(2<i>S</i>)-3,3-dimethyl-1-oxido-2-butyl]iminomethyl}phenolato)ethanol-<i>cis</i>-dioxomolybdenum(VI)
 at 100 K
;
_journal_coeditor_code           HG6292
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m275
_journal_page_last               m277
_journal_paper_doi               10.1107/S1600536806000146
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mo (C21 H32 N O2) O2 (C2 H6 O)]'
_chemical_formula_moiety         'C23 H38 Mo N O5'
_chemical_formula_sum            'C23 H38 Mo N O5'
_chemical_formula_weight         504.48
_chemical_name_systematic
;
(C)-(2,4-Di-tert-butyl-6-{[(2S)-3,3-dimethyl-1-oxido-2-
butyl]iminomethyl}phenolato)ethanol-cis-dioxomolybdenum(VI)
;
_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                   11.5961(4)
_cell_length_b                   19.9913(5)
_cell_length_c                   23.2143(6)
_cell_measurement_reflns_used    14425
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.459
_cell_measurement_theta_min      2.388
_cell_volume                     5381.6(3)
_computing_cell_refinement
;
CrysAlis RED-CCD (Oxford Diffraction, 2002)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2002)
;
_computing_data_reduction
;
CrysAlis RED-CCD
;
_computing_molecular_graphics
;
PLATON2002 (Spek, 2003) and ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur (TM) diffractometer with Sapphire CCD detector
;
_diffrn_measurement_method
;
rotation method data acquisition using \w
;
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35088
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.8740
_exptl_absorpt_correction_T_min  0.8293
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'(CrysAlis RED-CCD; Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.403
_refine_ls_abs_structure_details 'Flack (1983), 4802 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10881
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0315P)^2^+6.7957P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                10278
_reflns_number_total             10881
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6292.cif
_cod_data_source_block           I
_cod_database_code               2208078
_cod_database_fobs_code          2208078