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_4508073
_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) beta
;
_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                89.648(2)
_cell_angle_beta                 88.077(2)
_cell_angle_gamma                86.684(3)
_cell_formula_units_Z            2
_cell_length_a                   6.6894(2)
_cell_length_b                   7.9510(3)
_cell_length_c                   16.5450(4)
_cell_measurement_reflns_used    6868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5389
_cell_measurement_theta_min      3.6804
_cell_volume                     878.01(5)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w and \p scans'
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16692
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.70
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89570
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0507
_reflns_number_gt                2957
_reflns_number_total             3797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400782c_si_003.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4508073