(4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-{[2-(dimethylamino)ethyl]nitrilobis(methylene)}diphenolato)dioxidomolybdenum(VI) chloroform monosolvate
Lei, Xiangyang; Chelamalla, Nagasree; Acta Crystallographica Section E 67 (2011) m1510–; doi:10.1107/S160053681104092X

data_2232361
_publ_section_title
;
 (4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-{[2-(dimethylamino)ethyl]nitrilobis(methylene)}diphenolato)dioxidomolybdenum(VI)
 chloroform monosolvate
;
_journal_coeditor_code           JJ2100
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1510
_journal_paper_doi               10.1107/S160053681104092X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mo (C34 H54 N2 O2) O2], C H Cl3'
_chemical_formula_moiety         'C34 H54 Mo N2 O4, C H Cl3'
_chemical_formula_sum            'C35 H55 Cl3 Mo N2 O4'
_chemical_formula_weight         770.10
_chemical_name_systematic
;
(4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-{[2-
(dimethylamino)ethyl]nitrilobis(methylene)}diphenolato)dioxidomolybdenum(VI)
chloroform monosolvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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            4
_cell_length_a                   24.3475(10)
_cell_length_b                   13.9748(6)
_cell_length_c                   11.0267(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      62.70
_cell_measurement_theta_min      3.63
_cell_volume                     3751.9(3)
_computing_cell_refinement       '<i>FRAMBO</i> (Bruker, 1999)'
_computing_data_collection       '<i>FRAMBO</i> (Bruker, 1999)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker MWPC area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            79926
_diffrn_reflns_theta_full        59.98
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         4.82
_exptl_absorpt_coefficient_mu    5.124
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.1838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.506
_refine_ls_abs_structure_details 'Flack (1983), 2649 Friedel pairs'
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                5061
_reflns_number_total             5548
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2100.cif
_cod_data_source_block           I
_cod_database_code               2232361
_cod_database_fobs_code          2232361