Rhodium-catalyzed multiple C-H activation/highly <i>meta</i>-selective C-H amination between amidines and alkynes.
Xu, Fen; Song, Yuan-Yuan; Zhu, Wen-Jing; Liu, Chun-Sen; Lu, Ya-Zhou; Du, Miao; Chemical communications (Cambridge, England) 56 (2020) 11227–11230; doi:10.1039/d0cc04885b

data_7127074
_publ_section_title
;
 Rhodium-catalyzed multiple C-H activation/highly <i>meta</i>-selective
 C-H amination between amidines and alkynes.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11227
_journal_page_last               11230
_journal_paper_doi               10.1039/d0cc04885b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C23 H26 Cl N2 Rh, C7 H5 N'
_chemical_formula_sum            'C30 H31 Cl N3 Rh'
_chemical_formula_weight         571.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-26 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.426(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.7434(11)
_cell_length_b                   9.7093(4)
_cell_length_c                   22.2459(7)
_cell_measurement_reflns_used    4157
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      73.3620
_cell_measurement_theta_min      3.9910
_cell_volume                     5343.0(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9618
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.166
_diffrn_reflns_theta_min         3.573
_exptl_absorpt_coefficient_mu    6.255
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.660
_refine_diff_density_min         -3.043
_refine_diff_density_rms         0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.316
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.316
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.3161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3832
_reflns_number_total             4744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04885b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7127071--7127077.cif.'
_cod_database_code               7127074
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.340
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'