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_4113705
_publ_section_title
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 Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and
 Chromophoric Centers: Syntheses, Structures, and Electrochemistry
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_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_formula_moiety
;
 [Mo2 ((H3 C O C6 H4 N)2 C H)3 (O2 C C H C H2)]
;
_chemical_formula_sum            'C48 H48 Mo2 N6 O8'
_chemical_formula_weight         1028.80
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.9530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6216(10)
_cell_length_b                   16.9509(9)
_cell_length_c                   15.9886(9)
_cell_measurement_reflns_used    9514
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.510
_cell_measurement_theta_min      2.403
_cell_volume                     4568.3(4)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31386
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.142
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+3.0545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                8943
_reflns_number_total             10367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_12.cif
_cod_data_source_block           xl
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+3.0545P] 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^)+(0.0313P)^2^+3.0545P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4113705