Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and Chromophoric Centers: Syntheses, Structures, and Electrochemistry
F. Albert Cotton; James P. Donahue; Carlos A. Murillo; Journal of the American Chemical Society 125 (2003) 5436–5450; doi:10.1021/ja029101i

data_4113702
_publ_section_title
;
 Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and
 Chromophoric Centers: Syntheses, Structures, and Electrochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5436
_journal_page_last               5450
_journal_paper_doi               10.1021/ja029101i
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthesized
_chemical_formula_moiety
;
 [Mo2 (H3 C O C6 H4 N)2 C H)3 (H3 C C N)2] [(H5 C6)4 B]
;
_chemical_formula_sum            'C73 H71 B Mo2 N8 O6'
_chemical_formula_weight         1359.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.749(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7683(9)
_cell_length_b                   15.7031(13)
_cell_length_c                   38.653(3)
_cell_measurement_reflns_used    275
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.29
_cell_volume                     6533.0(9)
_computing_cell_refinement       'SAINT V. 6.02'
_computing_data_collection       'SMART V. 5.059'
_computing_data_reduction        'SAINT V. 6.02'
_computing_molecular_graphics    'SHELXTL V. 5.03 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'omega 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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            41243
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.40
_diffrn_standards_interval_count 'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.8675
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         15373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_obs          0.0622
_refine_ls_shift/esd_max         0.382
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+8.8557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1488
_refine_ls_wR_factor_obs         0.1286
_reflns_number_observed          9572
_reflns_number_total             15373
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_09.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+8.8557P] 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^)+(0.0481P)^2^+8.8557P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4113702