Polymorph of {2-[(2-hydroxyethyl)iminiomethyl]phenolato-κ<i>O</i>}dioxido{2-[(2-oxidoethyl)iminomethyl]phenolato-κ^3^<i>O</i>,<i>N</i>,<i>O</i>'}molybdenum(VI)
Agustin, Dominique; Jean-Claude Daran; Poli, Rinaldo; Acta Crystallographica Section C 64 (2008) m101–m104; doi:10.1107/S0108270108000127

data_2016456
_publ_section_title
;Polymorph of
 {2-[(2-hydroxyethyl)iminiomethyl]phenolato-\k<i>O</i>}dioxido{2-[(2-oxidoethyl)iminomethyl]phenolato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>'}molybdenum(VI)
;
_journal_coeditor_code           SK3193
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m101
_journal_page_last               m104
_journal_paper_doi               10.1107/S0108270108000127
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Mo (C9 H9 N O2) O2 (C9 H11 N O2)]'
_chemical_formula_moiety         'C18 H20 Mo N2 O6'
_chemical_formula_sum            'C18 H20 Mo N2 O6'
_chemical_formula_weight         456.30
_chemical_name_systematic
;
{2-[(2-hydroxyethyl)iminiomethyl]phenolato-\kO}dioxido(2-[(2-\
oxidoethyl)iminomethyl]phenolato-\k^3^O,N,O')molybdenum(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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                81.731(5)
_cell_angle_beta                 86.437(5)
_cell_angle_gamma                71.422(5)
_cell_formula_units_Z            6
_cell_length_a                   10.0953(5)
_cell_length_b                   13.5645(8)
_cell_length_c                   21.8864(14)
_cell_measurement_reflns_used    15657
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.91
_cell_measurement_theta_min      2.75
_cell_volume                     2810.9(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia,
1997),
CAMERON (Pearce <i>et al.</i>,  2000) and PLATON (Spek, 2003)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24992
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2007);
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm]
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.271
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         13844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0361P)^2^+4.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                10817
_reflns_number_total             13842
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3193.cif
_cod_data_source_block           I
_cod_database_code               2016456
_cod_database_fobs_code          2016456