<i>In Crystallo</i> Snapshots of Rh<sub>2</sub>-Catalyzed C-H Amination.
Das, Anuvab; Wang, Chen-Hao; Van Trieste, 3rd, Gerard P; Sun, Cheng-Jun; Chen, Yu-Sheng; Reibenspies, Joseph H.; Powers, David C.; Journal of the American Chemical Society 142 (2020) 19862–19867; doi:10.1021/jacs.0c09842

data_4135362
_publ_section_title
;
 <i>In Crystallo</i> Snapshots of Rh<sub>2</sub>-Catalyzed C-H Amination.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19862
_journal_page_last               19867
_journal_paper_doi               10.1021/jacs.0c09842
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C44 H49 N O8 Rh2, C H2 Cl2, N2'
_chemical_formula_sum            'C45 H51 Cl2 N3 O8 Rh2'
_chemical_formula_weight         1038.60
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9316(8)
_cell_length_b                   12.9312(9)
_cell_length_c                   32.433(2)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.93
_cell_measurement_theta_min      2.31
_cell_volume                     4524.3(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 2 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'Charge-integrating Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            115074
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.976
_diffrn_reflns_theta_min         0.988
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1415 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9244
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0534P)^2^+10.4943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7858
_reflns_number_total             9244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09842_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
Adding full bibliography for 4135359--4135363.cif.

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H102 Cl4 N6 O16 Rh4'
_cod_original_formula_weight         2077.21
_cod_original_formula_moiety         '2(C44 H49 N O8 Rh2), 2(C H2 Cl2), 2(N2)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4524.3(6)
_cod_database_code               4135362
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 N2-N1
 -3.1 with sigma of 0.02
3. Rigid bond restraints
 N2, N3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N2 \\sim N3: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C21(H21A,H21B), C28(H28A,H28B), C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C11(H11), C23(H23), C24(H24), C25(H25), C27(H27),
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              12969
_shelx_hkl_checksum              24502
_olex2_submission_special_instructions 'No special instructions were received'