Synthesis of 1-aminoisoquinolines via Rh(III)-catalyzed oxidative coupling.
Wei, Xiaohong; Zhao, Miao; Du, Zhengyin; Li, Xingwei; Organic letters 13 (2011) 4636–4639; doi:10.1021/ol2018505

data_1502412
_publ_section_title
;
 Synthesis of 1-aminoisoquinolines via Rh(III)-catalyzed oxidative
 coupling.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4636
_journal_page_last               4639
_journal_paper_doi               10.1021/ol2018505
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C46 H31 Cl3 N2'
_chemical_formula_weight         718.08
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.657(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.344(11)
_cell_length_b                   11.346(3)
_cell_length_c                   18.236(5)
_cell_measurement_reflns_used    3827
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48.272
_cell_measurement_theta_min      4.489
_cell_volume                     7321(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18124
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2075
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.165
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1497P)^2^+4.3441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2632
_reflns_number_gt                4200
_reflns_number_total             6786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol2018505_si_001.cif
_cod_data_source_block           cd211249
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7321(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1502412