Soluble Molybdenum(V) Imido Phthalocyanines and Pyrazinoporphyrazines: Crystal Structure, UV-vis and Electron Paramagnetic Resonance Spectroscopic Studies
Elisabeth Seikel; Benjamin Oelkers; Olaf Burghaus; Jörg Sundermeyer; Inorganic Chemistry 52 (2013) 4451–4457; doi:10.1021/ic3026914

data_4334475
_publ_section_title
;
 Soluble Molybdenum(V) Imido Phthalocyanines and Pyrazinoporphyrazines:
 Crystal Structure, UV-vis and Electron Paramagnetic Resonance
 Spectroscopic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4451
_journal_page_last               4457
_journal_paper_doi               10.1021/ic3026914
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C73 H83 Cl Mo N9, 4(C H2 Cl2)'
_chemical_formula_sum            'C77 H91 Cl9 Mo N9'
_chemical_formula_weight         1557.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           204
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   29.500(4)
_cell_length_b                   29.500(4)
_cell_length_c                   29.500(4)
_cell_measurement_reflns_used    923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.1
_cell_volume                     25672(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0809
_diffrn_reflns_av_sigmaI/netI    0.2303
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11783
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.9257
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             9732
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
 Heavily disordered dichloromethane near the origin
 could not be modeled satisfyingly and was thus removed
 using PLATON/SQUEEZE.
;
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.667
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      0.668
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                1727
_reflns_number_total             4773
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3026914_si_001.cif
_cod_data_source_block           es-pe-2
_cod_database_code               4334475