New Cyanometalate Building Units: Synthesis and Characterization of [Re(CN)7]3- and [Re(CN)8]3-
Miriam V. Bennett; Jeffrey R. Long; Journal of the American Chemical Society 125 (2003) 2394–2395; doi:10.1021/ja029795v

data_4113522
_publ_contact_author
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        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 New Cyanometalate Building Units: Synthesis and Characterization of
 [Re(CN)7]3- and [Re(CN)8]3-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2394
_journal_page_last               2395
_journal_paper_doi               10.1021/ja029795v
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_structural     (Bu4N)3Re(CN)7
_chemical_formula_sum            'C55 H108 N10 Re'
_chemical_formula_weight         1095.71
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.9918(3)
_cell_length_b                   23.0860(3)
_cell_length_c                   23.0773(5)
_cell_measurement_temperature    193(2)
_cell_volume                     12248.1(3)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.1080
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53436
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.249
_refine_ls_goodness_of_fit_obs   1.364
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         14922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_restrained_S_obs      1.364
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_obs          0.0541
_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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1489
_refine_ls_wR_factor_obs         0.1250
_reflns_number_observed          10110
_reflns_number_total             19272
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja029795v_s2_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] 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^)+(0.0459P)^2^+0.0000P] 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               4113522