Three Polymorphic Forms of a Monomeric Mo(VI) Complex: Building Blocks for Two Metal–Organic Supramolecular Isomers. Intermolecular Interactions and Ligand Substituent Effects
Vrdoljak, Višnja; Prugovečki, Biserka; Matković-Čalogović, Dubravka; Hrenar, Tomica; Dreos, Renata; Siega, Patrizia; Crystal Growth & Design 13 (2013) 3773–; doi:10.1021/cg400782c

data_4508074
_publ_section_title
;
 Three Polymorphic Forms of a Monomeric Mo(VI) Complex: Building Blocks
 for Two Metal--Organic Supramolecular Isomers. Intermolecular
 Interactions and Ligand Substituent Effects
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3773
_journal_paper_doi               10.1021/cg400782c
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C16 H17 Mo N3 O6'
_chemical_formula_weight         443.27
_chemical_name_systematic
;
ethanol(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato-O,O',N)-cis-
dioxomolybdenum(VI) gamma
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL-97
_cell_angle_alpha                87.511(11)
_cell_angle_beta                 83.424(12)
_cell_angle_gamma                87.411(13)
_cell_formula_units_Z            4
_cell_length_a                   8.2387(13)
_cell_length_b                   14.450(2)
_cell_length_c                   14.9022(18)
_cell_measurement_reflns_used    3263
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0965
_cell_measurement_theta_min      4.0655
_cell_volume                     1759.3(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2008)'
_computing_molecular_graphics    'PLATON98 (Spek, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21805
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66657
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.681
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         7615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                5257
_reflns_number_total             7615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400782c_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4508074