Neutral Macrocycles via Halide-Induced Ring Opening of Binuclear Condensed Intermediates
Felicia M. Dixon; Adam H. Eisenberg; Joshua R. Farrell; Chad A. Mirkin; Louise M. Liable-Sands; Arnold L. Rheingold; Inorganic Chemistry 39 (2000) 3432–3433; doi:10.1021/ic000062q

data_4321195
_publ_contact_author
; 
     Dr. C.A. Mirkin 
     Department of Chemistry 
     Northwestern University 
     2145 Sheridan Road 
     Evanston, Il  60208-3113 (USA) 
;
_publ_contact_author_email       camirkin@chem.nwu.edu
_publ_contact_author_fax         '+(847) 467-5123'
_publ_contact_author_phone       '+847 491 2907'
_publ_section_title
;
 Neutral Macrocycles via Halide-Induced Ring Opening of Binuclear
 Condensed Intermediates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3432
_journal_page_last               3433
_journal_paper_doi               10.1021/ic000062q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C126 H88 B2 F40 P4 Rh2 S4'
_chemical_formula_weight         2841.52
_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                91.9086(9)
_cell_angle_beta                 102.4122(7)
_cell_angle_gamma                96.2327(5)
_cell_formula_units_Z            1
_cell_length_a                   12.1280(2)
_cell_length_b                   15.7693(2)
_cell_length_c                   16.0488(2)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     2974.80(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.858
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21618
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.8204
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.431
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.431
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          2.332
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2152
_reflns_number_gt                10051
_reflns_number_total             12720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000062q_1.cif
_cod_data_source_block           mir24
_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_cell_volume        2974.80(6)
_cod_database_code               4321195