Crystal structure of aqua[(<i>E</i>)-<i>N</i>'-(5-bromo-2-oxidobenzylidene-κ<i>O</i>)benzohydrazidato-κ^2^<i>O</i>,<i>N</i>']dioxidomolybdenum(VI) dimethylformamide monosolvate
Sudheer, Radhika; Sithambaresan, M.; Sajitha, N. R.; Manoj, E.; Kurup, M. R. Prathapachandra; Acta Crystallographica Section E 71 (2015) 702–705; doi:10.1107/S2056989015009639

data_2240789
_publ_section_title
;
 Crystal structure of
 aqua[(<i>E</i>)-<i>N</i>'-(5-bromo-2-oxidobenzylidene-\k<i>O</i>)benzohydrazidato-\k^2^<i>O</i>,<i>N</i>']dioxidomolybdenum(VI)
 dimethylformamide monosolvate
;
_journal_coeditor_code           PK2550
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              702
_journal_page_last               705
_journal_paper_doi               10.1107/S2056989015009639
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Mo (C14 H9 Br N2 O2) O2 (H2 O)], C3 H7 N O'
_chemical_formula_moiety         'C14 H11 Br Mo N2 O5, C3 H7 N O'
_chemical_formula_sum            'C17 H18 Br Mo N3 O6'
_chemical_formula_weight         536.19
_chemical_name_systematic
;Aqua[(<i>E</i>)-<i>N</i>'-(5-bromo-2-oxidobenzylidene-\k<i>O</i>)benzohydrazidato-\k^2^<i>O</i>,<i>N</i>']dioxidomolybdenum(VI)
dimethylformamide monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.900(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8581(8)
_cell_length_b                   7.1145(5)
_cell_length_c                   25.998(2)
_cell_measurement_reflns_used    5189
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.105
_cell_measurement_theta_min      2.863
_cell_volume                     2003.7(3)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2004)
;
_computing_molecular_graphics
;
ORTEP-3 (Burnett & Johnson, 1996) and DIAMOND (Brandenburg,
2010)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         2.913
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  0.4470
_exptl_absorpt_correction_T_min  0.3550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.885
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0418P)^2^+1.3003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                3710
_reflns_number_total             4957
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2550sup1.cf
_cod_data_source_block           I
_cod_database_code               2240789
_cod_database_fobs_code          2240789
_shelx_estimated_absorpt_t_min   0.413
_shelx_estimated_absorpt_t_max   0.499
_shelx_hkl_checksum              71960
_shelx_res_checksum              86014
_shelxl_version_number           2.014