A cocrystal of two Mo^VI^ complexes bearing different diastereomers of the 2,4-di-<i>tert</i>-butyl-6-{[(1-oxido-1-phenylpropan-2-yl)(methyl)amino]methyl}phenolate ligand derived from (+)-ephedrine
Sillanpää, Reijo; Hänninen, Mikko M.; Acta Crystallographica Section C 69 (2013) 509–512; doi:10.1107/S0108270113010652

data_2018973
_publ_section_title
;
 A cocrystal of two Mo^VI^ complexes bearing different diastereomers of
 the
 2,4-di-<i>tert</i>-butyl-6-{[(1-oxido-1-phenylpropan-2-yl)(methyl)amino]methyl}phenolate
 ligand derived from (+)-ephedrine
;
_journal_coeditor_code           LG3109
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              509
_journal_page_last               512
_journal_paper_doi               10.1107/S0108270113010652
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Mo (C25 H35 N O2) O2 (C H4 O)]'
_chemical_formula_moiety         'C26 H39 Mo N O5'
_chemical_formula_sum            'C26 H39 Mo N O5'
_chemical_formula_weight         541.52
_chemical_name_systematic
;
[(1<i>S</i>,2<i>R</i>,<i>R</i>~N~)-2,4-Di-<i>tert</i>-butyl-6-{[(1-oxido-1-\
phenylpropan-2-yl)(methyl)amino]methyl}phenolato](methanol)-<i>cis</i>-\
dioxidomolybdenum(VI)--[(1<i>S</i>,2<i>R</i>,<i>S</i>~N~)-2,4-di-<i>tert</i>-\
butyl-6-{[(1-oxido-1-phenylpropan-2-\
yl)(methyl)amino]methyl}phenolato](methanol)-<i>cis</i>-dioxidomolybdenum(VI)
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 109.9340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1560(4)
_cell_length_b                   8.41290(10)
_cell_length_c                   20.3545(6)
_cell_measurement_reflns_used    4502
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      0.407
_cell_volume                     2600.80(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999) and <i>Mercury</i> (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15118
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.544
_refine_ls_abs_structure_details 'Flack (1983), with 4298 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.3404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.082
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                8963
_reflns_number_total             9756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3109.cif
_cod_data_source_block           I
_cod_original_cell_volume        2600.80(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018973
_cod_database_fobs_code          2018973