Characterization of a Reactive Rh<sub>2</sub> Nitrenoid by Crystalline Matrix Isolation.
Das, Anuvab; Chen, Yu-Sheng; Reibenspies, Joseph H.; Powers, David C.; Journal of the American Chemical Society 141 (2019) 16232–16236; doi:10.1021/jacs.9b09064

data_4127693
_publ_section_title
;
 Characterization of a Reactive Rh<sub>2</sub> Nitrenoid by Crystalline
 Matrix Isolation.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16232
_journal_page_last               16236
_journal_paper_doi               10.1021/jacs.9b09064
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'2(C42 H56 N O9 Rh2), 2(C42 H57 N O9 Rh2), 4(C H Cl3)'
_chemical_formula_sum            'C172 H230 Cl12 N4 O36 Rh8'
_chemical_formula_weight         4178.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.875(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6255(10)
_cell_length_b                   21.4629(10)
_cell_length_c                   22.5422(11)
_cell_measurement_reflns_used    9206
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.21
_cell_volume                     8929.7(8)
_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 0.999
_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  0.1052
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            211133
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         2.127
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1187 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.8964.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4284
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         18287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0189P)^2^+39.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14467
_reflns_number_total             18287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09064_si_002.cif
_cod_data_source_block           5a
_cod_database_code               4127693
_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, All C(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,
  H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2), C3(H3), C5(H5), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B), C19(H19A,H19B), C26(H26A,H26B), C35(H35A,H35B),
 C42(H42A,H42B), C51(H51A,H51B), C58(H58A,H58B), C2(H2A,H2B), C4(H4A,H4B),
 C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C9(H9), C21(H21), C23(H23), C24(H24), C25(H25),
 C37(H37), C39(H39), C40(H40), C41(H41), C53(H53), C55(H55), C56(H56), C57(H57)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O10(H10)
;
_shelx_res_checksum              89767
_shelx_hkl_checksum              46709
_olex2_submission_special_instructions 'No special instructions were received'