Synthesis and Properties of Rhenium Carbonyl Complexes of α,α'-Bis[(1-pyrenyl)pyrazol-1-yl]alkane Ligands
Daniel L. Reger; James R. Gardinier; Perry J. Pellechia; Mark D. Smith; Kenneth J. Brown; Inorganic Chemistry 42 (2003) 7635–7643; doi:10.1021/ic034631g

data_4312492
_publ_section_title
;
 Synthesis and Properties of Rhenium Carbonyl Complexes of
 \a,\a'-Bis[(1-pyrenyl)pyrazol-1-yl]alkane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7635
_journal_page_last               7643
_journal_paper_doi               10.1021/ic034631g
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
; 
[Re Br (C45 H30 N4 O3)] 0.25(C3 H6 O), 0.25(C4 H10 O) 
;
_chemical_formula_sum            'C46.75 H34 Br N4 O3.5 Re'
_chemical_formula_weight         973.89
_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                66.333(2)
_cell_angle_beta                 78.312(2)
_cell_angle_gamma                83.869(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6491(8)
_cell_length_b                   14.6714(13)
_cell_length_c                   17.2380(16)
_cell_measurement_reflns_used    5195
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      23.263
_cell_measurement_theta_min      2.089
_cell_volume                     1961.1(3)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13374
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.166
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.366
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                4617
_reflns_number_total             5656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034631gsi20030606_114842_1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C46.75 H34 Br N4 O3.50 Re'
_cod_database_code               4312492