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_4322168
_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            'C44.9 H29.8 Cl2.8 Mo N4 O5'
_chemical_formula_weight         900.53
_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                89.150(10)
_cell_angle_beta                 108.860(10)
_cell_angle_gamma                103.96(2)
_cell_formula_units_Z            2
_cell_length_a                   11.437(2)
_cell_length_b                   13.537(6)
_cell_length_c                   13.764(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1952.4(11)
_computing_cell_refinement       madnes
_computing_data_collection       madnes
_computing_data_reduction        'Madnes (Messerschmidt & 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      293(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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18920
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        'No measurable crystal decay'
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Rectangle
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_obs          0.0426
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.7341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1124
_refine_ls_wR_factor_obs         0.1082
_reflns_number_observed          8443
_reflns_number_total             9430
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990566s_1.cif
_cod_data_source_block           sd:cheng1
_cod_depositor_comments
;
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^)+(0.0505P)^2^+1.7341P] 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^)+(0.0505P)^2^+1.7341P] 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        'C44.90 H29.80 Cl2.80 Mo N4 O5'
_cod_database_code               4322168