<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_4135361
_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         '2(C88 H98 N2 O16 Rh4), 8(C H Cl3)'
_chemical_formula_sum            'C184 H204 Cl24 N4 O32 Rh8'
_chemical_formula_weight         4657.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                111.577(2)
_cell_angle_beta                 94.521(2)
_cell_angle_gamma                96.215(2)
_cell_formula_units_Z            1
_cell_length_a                   15.6237(9)
_cell_length_b                   17.2551(8)
_cell_length_c                   19.6274(13)
_cell_measurement_reflns_used    9549
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.75
_cell_volume                     4851.2(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      110(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'Bruker SMART CCD APEX2 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD APEX2 area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            286378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.125
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1522 before and 0.0923 after correction.
The Ratio of minimum to maximum transmission is 0.7984.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1159
_refine_ls_number_reflns         19846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_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^+10.9478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17423
_reflns_number_total             19846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09842_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 4135359--4135363.cif.'
_cod_database_code               4135361
_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.a Ternary CH refined with riding coordinates:
 C45(H45), C46(H46), C92(H92), C91(H91)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C21(H21A,H21B), C28(H28A,H28B), C51(H51A,H51B),
 C58(H58A,H58B), C67(H67A,H67B), C74(H74A,H74B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C11(H11), C23(H23), C24(H24), C25(H25), C27(H27),
 C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43),
  C53(H53), C54(H54), C55(H55), C57(H57), C69(H69), C70(H70), C71(H71),
 C73(H73), C80(H80), C81(H81), C82(H82), C83(H83), C86(H86), C87(H87), C88(H88),
  C89(H89)
2.d 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), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C)
;
_shelx_res_checksum              26221
_shelx_hkl_checksum              15682
_olex2_submission_special_instructions 'No special instructions were received'