New Mo(IV) complex with the pentadentate (N3O2) Schiff-base ligand: The first non-cyanide pentagonal-bipyramidal paramagnetic 4d complex
Mironov, Vladimir Sergeevich; Bazhenova, Tamara A.; Manakin, Yuriy; Lyssenko, Konstantin; Talantsev, Artem Dmitrievich; Yagubskii, Eduard B.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02912H

data_7044266
_publ_section_title
;
 New Mo(IV) complex with the pentadentate (N3O2) Schiff-base ligand: The
 first non-cyanide pentagonal-bipyramidal paramagnetic 4d complex
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02912H
_journal_year                    2017
_chemical_formula_moiety         'C23 H19 Cl2 Mo N5 O2, C H Cl3'
_chemical_formula_sum            'C24 H20 Cl5 Mo N5 O2'
_chemical_formula_weight         683.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.494(3)
_cell_length_b                   13.523(3)
_cell_length_c                   14.425(3)
_cell_measurement_reflns_used    944
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     2632.3(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.064
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_transmission_factor_max   0.843
_exptl_transmission_factor_min   0.739
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2584 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+0.9448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6271
_reflns_number_total             6999
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c7dt02912h2.cif
_cod_data_source_block           1
_cod_database_code               7044266
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.843
_shelxl_version_number           2014/6
_shelx_res_checksum              41722