Bis[(2,3,6,7,12,13,16,17-octaethylporphycenato)oxomolybdenum(V)] hexamolybdate(VI)
Maeda, Daisuke; Aritome, Isao; Shimakoshi, Hisashi; Hisaeda, Yoshio; Acta Crystallographica Section E 62 (2006) m1272–m1274; doi:10.1107/S1600536806016461

data_2209184
_publ_section_title
;
 Bis[(2,3,6,7,12,13,16,17-octaethylporphycenato)oxomolybdenum(V)]
 hexamolybdate(VI)
;
_journal_coeditor_code           HB2046
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1272
_journal_page_last               m1274
_journal_paper_doi               10.1107/S1600536806016461
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mo (C36 H44 N4) O]2 [Mo6 O19]'
_chemical_formula_moiety         '2C36 H44 Mo N4 O +, Mo6 O19 2-'
_chemical_formula_sum            'C72 H88 Mo8 N8 O21'
_chemical_formula_weight         2169.02
_chemical_name_common            'Mo(V)(O)(OEPc) 0.5(Mo6O19)'
_chemical_name_systematic
;
Bis[(2,3,6,7,12,13,16,17-octaethylporphycenato)oxomolybdenum(V)]
hexamolybdate
;
_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                62.426(2)
_cell_angle_beta                 77.652(2)
_cell_angle_gamma                79.594(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5979(11)
_cell_length_b                   13.4762(13)
_cell_length_c                   14.5563(15)
_cell_measurement_reflns_used    2294
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.77
_cell_measurement_theta_min      2.58
_cell_volume                     1961.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\p and \w'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11847
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  418
_diffrn_standards_number         88
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.928
_refine_diff_density_min         -0.738
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                4809
_reflns_number_total             7157
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2046.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2209184
_cod_database_fobs_code          2209184