Azide alkyne cycloaddition facilitated by hexanuclear rhenium chalcogenide cluster complexes.
Knott, Stanley A.; Templeton, Jeffrey N.; Durham, Jessica L.; Howard, Angela M.; McDonald, Robert; Szczepura, Lisa F.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8132–8139; doi:10.1039/c3dt50436k

data_7022970
_publ_section_title
;
 Azide alkyne cycloaddition facilitated by hexanuclear rhenium
 chalcogenide cluster complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8132
_journal_page_last               8139
_journal_paper_doi               10.1039/c3dt50436k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C30 H75 N3 P5 Re6 Se8, 3(C4 H10 O), B F4'
_chemical_formula_sum            'C42 H105 B F4 N3 O3 P5 Re6 Se8'
_chemical_formula_weight         2690.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 92.6900(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5343(8)
_cell_length_b                   20.3729(11)
_cell_length_c                   19.5681(11)
_cell_measurement_reflns_used    5606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.25
_cell_volume                     6186.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27372
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.582
_exptl_absorpt_correction_T_max  0.2879
_exptl_absorpt_correction_T_min  0.0774
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as
disordered or partial-occupancy solvent diethyl ether oxygen or carbon
atoms were unsuccessful. The data were corrected for disordered
electron density through use of the SQUEEZE procedure (Sluis, P. van
der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented
in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L.
J. Appl. Cryst. 2003, 36, 7-13. PLATON - a multipurpose
crystallographic tool. Utrecht University, Utrecht, The Netherlands).
A total solvent-accessible void volume of 877.7 cubic Angstroms with a
total electron count of 591 (consistent with 12 molecules of solvent
diethyl ether, or 3 molecules per formula unit of the hexarhenium
complex ion) was found in the unit cell.
;
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         14247
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0320P)^2^+14.7434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                12351
_reflns_number_total             14247
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50436k.txt
_cod_data_source_block           isu1102
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7022970