An Efficient Synthesis of Acetylide/Trimetal/Acetylide Molecular Wires
John F. Berry; F. Albert Cotton; Carlos A. Murillo; Brian K. Roberts; Inorganic Chemistry 43 (2004) 2277–2283; doi:10.1021/ic0354320

data_4310814
_publ_section_title
;
 An Efficient Synthesis of Acetylide/Trimetal/Acetylide Molecular Wires
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2277
_journal_page_last               2283
_journal_paper_doi               10.1021/ic0354320
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'Co3(C10H8N3)4(NC2H3)(C8H5), PF6, (C4H8O)3.95'
_chemical_formula_sum            'C65.8 H71.6 Co3 F6 N13 O3.95 P'
_chemical_formula_weight         1429.52
_chemical_melting_point          ?
_chemical_name_common            '[Co3(dpa)4(NCMe)2(CCPh)2]PF6, 3.95THF'
_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-97
_cell_angle_alpha                73.289(4)
_cell_angle_beta                 65.744(4)
_cell_angle_gamma                77.236(4)
_cell_formula_units_Z            2
_cell_length_a                   15.409(3)
_cell_length_b                   16.297(3)
_cell_length_c                   16.340(3)
_cell_measurement_reflns_used    2214
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48
_cell_measurement_theta_min      5
_cell_volume                     3558.1(12)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w-scan
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11307
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.8466
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         9584
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1756
_reflns_number_gt                5321
_reflns_number_total             9584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354320si20031213_044610_2.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z 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 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        3558.2(12)
_cod_original_formula_sum        'C65.80 H71.60 Co3 F6 N13 O3.95 P'
_cod_database_code               4310814