Molybdenum(V) on an Oxide String. Synthesis and Structure of the Novel Linear Trinuclear Complex {[MoO(TPP)][O-Mo(TPP)-O][MoO(TPP)]}ClO4
Brent J. Hamstra; Beisong Cheng; Mary K. Ellison; W. Robert Scheidt; Inorganic Chemistry 38 (1999) 3554–3561; doi:10.1021/ic990566s

data_4322169
_publ_section_title
;
 Molybdenum(V) on an Oxide String. Synthesis and Structure of the Novel
 Linear Trinuclear Complex {[MoO(TPP)][O-Mo(TPP)-O][MoO(TPP)]}ClO4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3554
_journal_page_last               3561
_journal_paper_doi               10.1021/ic990566s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C54.5 H42 Cl Mo N4 O6'
_chemical_formula_weight         980.31
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                74.292(8)
_cell_angle_beta                 69.114(8)
_cell_angle_gamma                69.030(5)
_cell_formula_units_Z            2
_cell_length_a                   13.2138(7)
_cell_length_b                   13.5959(12)
_cell_length_c                   14.6676(11)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     2267.7(3)
_computing_cell_refinement       madnes
_computing_data_collection       madnes
_computing_data_reduction        'Madnes (Messerschmitt & Pflugraph, 1987)'
_computing_molecular_graphics    'Ortep III (Burnett, Johnson, 1996)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_measurement_device       'Enraf-Nonius fast area-detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22144
_diffrn_reflns_theta_max         29.85
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        'No measurable crystal decay'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Rectangle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_obs          0.0488
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.9398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1145
_refine_ls_wR_factor_obs         0.1087
_reflns_number_observed          10045
_reflns_number_total             11482
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990566s_2.cif
_cod_data_source_block           sd:cheng2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.9398P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.9398P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C54.50 H42 Cl Mo N4 O6'
_cod_database_code               4322169