RhCl(PPh3)3-mediated C-H oxyfunctionalization of pyrrolido-functionalized bisazoaromatic pincers: a combined experimental and theoretical scrutiny of redox-active and spectroscopic properties.
Ghorui, Tapas; Roy, Sima; Pramanik, Shuvam; Pramanik, Kausikisankar; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5720–5729; doi:10.1039/c5dt05044h

data_7038472
_publ_section_title
;
 RhCl(PPh3)3-mediated C-H oxyfunctionalization of pyrrolido-functionalized
 bisazoaromatic pincers: a combined experimental and theoretical scrutiny
 of redox-active and spectroscopic properties.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5720
_journal_page_last               5729
_journal_paper_doi               10.1039/c5dt05044h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C110 H81 Br4 Cl2 N13 O2 P4 Rh2'
_chemical_formula_weight         2337.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-12 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.4850(11)
_cell_length_b                   16.3476(5)
_cell_length_c                   19.3520(6)
_cell_measurement_reflns_used    105473
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.352
_cell_measurement_theta_min      2.328
_cell_volume                     9828.7(5)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            153092
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.352
_diffrn_reflns_theta_min         2.328
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown-green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.273
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.00034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         24426
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+55.6622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19151
_reflns_number_total             24426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt05044h2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7038472.cif.'
_cod_database_code               7038472
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.467
_shelx_estimated_absorpt_t_max   0.639
_shelx_res_checksum              83736