Half-sandwich (η<sup>5</sup>-Cp*)Rh(iii) complexes of pyrazolated organo-sulfur/selenium/tellurium ligands: efficient catalysts for base/solvent free C-N coupling of chloroarenes under aerobic conditions.
Sharma, Charu; Srivastava, Avinash Kumar; Sharma, Kamal Nayan; Joshi, Raj Kumar; Organic & biomolecular chemistry 18 (2020) 3599–3606; doi:10.1039/d0ob00538j

data_7157477
_publ_section_title
;
 Half-sandwich (\h<sup>5</sup>-Cp*)Rh(iii) complexes of pyrazolated
 organo-sulfur/selenium/tellurium ligands: efficient catalysts for
 base/solvent free C-N coupling of chloroarenes under aerobic conditions.
;
_journal_issue                   18
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3599
_journal_page_last               3606
_journal_paper_doi               10.1039/d0ob00538j
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C21 H26 Br Cl N2 Rh S, F6 P'
_chemical_formula_sum            'C21 H26 Br Cl F6 N2 P Rh S'
_chemical_formula_weight         701.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-02 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.874(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.562(3)
_cell_length_b                   11.151(2)
_cell_length_c                   19.041(4)
_cell_measurement_reflns_used    5351
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.25
_cell_volume                     2665.8(10)
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11514
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.140
_exptl_absorpt_coefficient_mu    2.433
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile and methanol'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.758
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 1770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4650
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+4.5968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4142
_reflns_number_total             4650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00538j2.cif
_cod_data_source_block           Complex1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7157476--7157477.cif.'
_cod_original_cell_volume        2666.1(9)
_cod_database_code               7157477
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.108
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'