Stepwise Formation of a Molecular Square with Bridging NH,O-Substituted Dicarbene Building Blocks
Fabian M. Conrady; Roland Fröhlich; Christian Schulte to Brinke; Tania Pape; F. Ekkehardt Hahn; Journal of the American Chemical Society 133 (2011) 11496–11499; doi:10.1021/ja205021p

data_4106482
_publ_section_title
;
 Stepwise Formation of a Molecular Square with Bridging NH,O-Substituted
 Dicarbene Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11496
_journal_page_last               11499
_journal_paper_doi               10.1021/ja205021p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C72 H76 Cl8 Ir4 N8 O8'
_chemical_formula_weight         2233.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9760(4)
_cell_length_b                   16.9760(4)
_cell_length_c                   43.550(2)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     12550.4(7)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            47853
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.434
_exptl_absorpt_correction_T_max  0.8426
_exptl_absorpt_correction_T_min  0.6910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.523237  

;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       'transaprent prism'
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.783
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         6407
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0762
_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^)+(0.0893P)^2^+146.5908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                4953
_reflns_number_total             6407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205021p_si_004.cif
_cod_data_source_block           sad
_cod_original_cell_volume        12550.5(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4106482