A sustainable catalytic pyrrole synthesis
Stefan Michlik; Rhett Kempe; Nature Chemistry 5 (2013) 140–144; doi:10.1038/nchem.1547

data_1551875
_publ_section_title
;
 A sustainable catalytic pyrrole synthesis
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              140
_journal_page_last               144
_journal_paper_doi               10.1038/nchem.1547
_journal_volume                  5
_journal_year                    2013
_chemical_formula_sum            'C29 H46 Ir N5 P2'
_chemical_formula_weight         718.85
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.8530(11)
_cell_length_b                   42.232(2)
_cell_length_c                   14.7820(12)
_cell_measurement_reflns_used    22085
_cell_measurement_temperature    133(2)
_cell_volume                     12393.7(14)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-RED32
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_sigmaI/netI    0.0946
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19287
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  0.2351
_exptl_absorpt_correction_T_min  0.1283
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.759
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5231
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                3973
_reflns_number_total             5231
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            nchem.1547-s2.cif
_cod_data_source_block           t257ofma1
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               1551875
_cell_measurement_2theta_min     3.56
_cell_measurement_2theta_max     45.95