Templated C-C and C-N Bond Formation Facilitated by a Molybdenum(VI) Metal Center.
Zwettler, Niklas; Dupé, Antoine; Schachner, Jörg A; Belaj, Ferdinand; Mösch-Zanetti, Nadia C; Inorganic chemistry 54 (2015) 11969–11976; doi:10.1021/acs.inorgchem.5b02347

data_4346909
_publ_section_title
;
 Templated C-C and C-N Bond Formation Facilitated by a Molybdenum(VI)
 Metal Center.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11969
_journal_page_last               11976
_journal_paper_doi               10.1021/acs.inorgchem.5b02347
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C26 H40 Mo N2 O6, C2 H3 N'
_chemical_formula_sum            'C28 H43 Mo N3 O6'
_chemical_formula_weight         613.59
_chemical_name_common
; (4,6-di-tert-butyl-6-[(E)-({2-methyl-1-[(methylamino)carbonyl]-2-oxi-
do-4-oxopentyl}imino)methyl]benzenolato-N,O,O',O")-dioxo-molybdenum(VI)
acetonitrile solvate (1:1)
;
_chemical_name_systematic
; (4,6-di-tert-butyl-6-[(E)-({2-methyl-1-[(methylamino)carbonyl]-2-oxi-
do-4-oxopentyl}imino)methyl]benzenolato-N,O,O',O")-dioxo-molybdenum(VI)
acetonitrile solvate (1:1)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.3972(13)
_cell_length_b                   7.9229(4)
_cell_length_c                   34.2903(19)
_cell_measurement_reflns_used    9156
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.38
_cell_volume                     6084.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            52561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       needle
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.715
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8863
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+1.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6751
_reflns_number_total             8863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02347_si_002.cif
_cod_data_source_block           5_NZ132P
_cod_database_code               4346909
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2014/6
_shelx_res_checksum              95078
_shelx_hkl_checksum              31402