Cp*Rh(iii)-catalyzed electrophilic amination of arylboronic acids with azo compounds for synthesis of arylhydrazides.
Lau, Yan-Fung; Chan, Chun-Ming; Zhou, Zhongyuan; Yu, Wing-Yiu; Organic & biomolecular chemistry 14 (2016) 6821–6825; doi:10.1039/c6ob00719h

data_7155164
_publ_section_title
;
 Cp*Rh(iii)-catalyzed electrophilic amination of arylboronic acids with
 azo compounds for synthesis of arylhydrazides.
;
_journal_issue                   28
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6821
_journal_page_last               6825
_journal_paper_doi               10.1039/c6ob00719h
_journal_volume                  14
_journal_year                    2016
_chemical_formula_sum            'C34 H35 Br P Rh'
_chemical_formula_weight         657.41
_chemical_name_systematic
'Rhodium,bromo-(1,2,3,4,5-pentamethylcyclopentadienyl)phenyl(triphenylphosphine) complex'
_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
_audit_update_record
;
2016-05-12 deposited with the CCDC.
2016-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                104.905(2)
_cell_angle_beta                 100.8330(10)
_cell_angle_gamma                98.7530(10)
_cell_formula_units_Z            4
_cell_length_a                   10.4383(2)
_cell_length_b                   15.6767(4)
_cell_length_c                   19.2505(5)
_cell_measurement_reflns_used    7965
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.04
_cell_measurement_theta_min      2.27
_cell_volume                     2922.39(13)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80719
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SAINT ver 7.34; Bruker SADABS'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.184
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13409
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+34.1308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2502
_reflns_number_gt                7637
_reflns_number_total             13409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob00719h2.cif
_cod_data_source_block           lyf5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7155163--7155166.cif.
;
_cod_original_cell_volume        2922.39(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7155164