Controlling the Addition of Metal Centers to a Bis(pyrazolyl)methane Starburst Ligand: Direct Routes to Mono-, Bi-, and Trimetallic Rhenium(I) Complexes
Reger, Daniel L.; Watson, Russell P.; Smith, Mark D.; Pellechia, Perry J.; Organometallics 25 (2006) 743–; doi:10.1021/om0508684

data_4074769
_publ_section_title
;
 Controlling the Addition of Metal Centers to a Bis(pyrazolyl)methane
 Starburst Ligand:&#x00A0; Direct Routes to Mono-, Bi-, and Trimetallic
 Rhenium(I) Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              743
_journal_paper_doi               10.1021/om0508684
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C36 H24 Br3 N12 O9 Re3, 4.5(C3 H6 O)'
_chemical_formula_sum            'C49.5 H51 Br3 N12 O13.5 Re3'
_chemical_formula_weight         1828.35
_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                95.9450(10)
_cell_angle_beta                 96.2050(10)
_cell_angle_gamma                117.6460(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2164(8)
_cell_length_b                   14.1142(9)
_cell_length_c                   19.1630(12)
_cell_measurement_reflns_used    8621
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.398
_cell_measurement_theta_min      2.232
_cell_volume                     3099.6(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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32478
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    7.844
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.315
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         12705
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+13.7572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                10694
_reflns_number_total             12705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0508684si20051007_114323.cif
_cod_data_source_block           6rw720cs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C49.50 H51 Br3 N12 O13.50 Re3'
_cod_database_code               4074769