NO• Disproportionation by a {RhNO}9 Pincer-Type Complex
Gaviglio, Carina; Pellegrino, Juan; Milstein, David; Doctorovich, Fabio; Dalton Transactions  (2017) –; doi:10.1039/C7DT03944A

data_7044797
_publ_section_title
;
 NO&#x2022; Disproportionation by a {RhNO}9 Pincer-Type Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03944A
_journal_year                    2017
_chemical_formula_moiety         'C26 H47 N2 O3 P2 Rh'
_chemical_formula_sum            'C26 H47 N2 O3 P2 Rh'
_chemical_formula_weight         600.50
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-10-13 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.098(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6789(2)
_cell_length_b                   23.1826(5)
_cell_length_c                   14.3797(3)
_cell_measurement_reflns_used    13405
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.7290
_cell_measurement_theta_min      3.7380
_cell_volume                     2885.79(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1158
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
  1 omega  -49.00   45.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145  -57.0000   30.0000 94

  2 omega   32.00  103.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145 -178.0000  120.0000 71

  3 omega  -12.00   94.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145   77.0000 -150.0000 106

  4 omega  -49.00   45.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145  -57.0000   90.0000 94

  5 omega  -25.00   23.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  -99.0000 -120.0000 48

  6 omega  -92.00    2.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  -57.0000 -180.0000 94

  7 omega  -45.00   49.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052   57.0000  -30.0000 94

  8 omega  -25.00   23.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  -99.0000  -90.0000 48

  9 omega -104.00  -53.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  178.0000  -30.0000 51

 10 omega   -2.00   92.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145   57.0000   60.0000 94

 11 omega  -25.00   39.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145  -99.0000 -150.0000 64

 12 omega   -2.00   92.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145   57.0000    0.0000 94

 13 omega   35.00  101.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -       21.2145  178.0000  -60.0000 66

 14 omega -104.00  -53.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  178.0000  120.0000 51

 15 omega  -25.00   23.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  -99.0000   90.0000 48

 16 omega  -92.00    2.00   1.0000    2.1050
omega____ theta____ kappa____ phi______ frames
    -      -21.6052  -57.0000   60.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0040288000
_diffrn_orient_matrix_UB_12      -0.0085885000
_diffrn_orient_matrix_UB_13      -0.0471022000
_diffrn_orient_matrix_UB_21      0.0271484000
_diffrn_orient_matrix_UB_22      -0.0275687000
_diffrn_orient_matrix_UB_23      0.0150206000
_diffrn_orient_matrix_UB_31      -0.0771860000
_diffrn_orient_matrix_UB_32      -0.0101412000
_diffrn_orient_matrix_UB_33      -0.0009039000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.111
_diffrn_reflns_theta_min         3.664
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Oxford Diffraction (2009)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         7231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5645
_reflns_number_total             7231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03944a2.cif
_cod_data_source_block           exp_4178
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2885.79(12)
_cod_database_code               7044797
_chemical_oxdiff_formula         'C26 H47 N2 O3 P2 Rh1'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C10(H10A,H10B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C14(H14A,H14B,
 H14C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C7(H7A,
 H7B,H7C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C16(H16A,
 H16B,H16C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              99341
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'