Dioxidomolybdenum(VI) complex featuring a 2,4-difluoro-substituted amine bis(phenolate) ligand
Bowen, Christina L.; Wile, Bradley M.; IUCrData 6 (2021) x210516–; doi:10.1107/S2414314621005162

data_1562819
_publ_section_title
;
 Dioxidomolybdenum(VI) complex featuring a 2,4-difluoro-substituted amine
 bis(phenolate) ligand
;
_journal_coeditor_code           PK4033
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x210516
_journal_paper_doi               10.1107/S2414314621005162
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          '[Mo (C18 H18 F4 N2 O2) O2]'
_chemical_formula_moiety         'C18 H18 F4 Mo N2 O4'
_chemical_formula_sum            'C18 H18 F4 Mo N2 O4'
_chemical_formula_weight         498.28
_chemical_name_systematic
'[2,2'-({[2-(Dimethylamino)ethyl]azanediyl}bis(methylene))bis(4,6-difluorophenolato)]dioxidomolybdenum(VI))'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                91.8513(18)
_cell_angle_beta                 92.9102(18)
_cell_angle_gamma                116.6842(16)
_cell_formula_units_Z            2
_cell_length_a                   7.3179(4)
_cell_length_b                   8.0093(4)
_cell_length_c                   17.5057(9)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.2153
_cell_measurement_theta_min      2.3344
_cell_volume                     913.82(8)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b),
<i>ShelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.254
_diffrn_reflns_theta_min         2.852
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.478
_refine_ls_extinction_coef       0.0171(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2018/3</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.4598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                6541
_reflns_number_total             7013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk4033sup1.cif
_cod_data_source_block           I
_cod_database_code               1562819
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.891
_shelx_hkl_checksum              88548
_shelx_res_checksum              25048
_cod_database_fobs_code 1562819