Synthesis, structure and reactivity of NO<sup>+</sup>, NO˙ and NO<sup>-</sup> pincer PCN-Rh complexes.
Gallego, Cecilia Mariel; Gaviglio, Carina; Ben-David, Yehoshoa; Milstein, David; Doctorovich, Fabio; Pellegrino, Juan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7093–7108; doi:10.1039/d0dt00962h

data_7704298
_publ_section_title
;
 Synthesis, structure and reactivity of NO<sup>+</sup>, NO&#x02D9; and
 NO<sup>-</sup> pincer PCN-Rh complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7093
_journal_page_last               7108
_journal_paper_doi               10.1039/d0dt00962h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H35 Cl N2 O P Rh'
_chemical_formula_sum            'C20 H35 Cl N2 O P Rh'
_chemical_formula_weight         488.83
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-12 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.744(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8734(5)
_cell_length_b                   15.0578(6)
_cell_length_c                   14.9966(7)
_cell_measurement_reflns_used    6563
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4750
_cell_measurement_theta_min      3.9850
_cell_volume                     2296.21(19)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1158
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
  1 omega  -56.00   55.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -       16.8217  -19.0000  150.0000 111

  2 omega   35.00   91.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -       16.8217  178.0000   60.0000 56

  3 omega  -25.00   23.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -      -17.2514  -99.0000    0.0000 48

  4 omega  -36.00   51.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -      -17.2514   57.0000 -120.0000 87

  5 omega  -54.00   39.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -       16.8217  -37.0000   60.0000 93

  6 omega   -2.00   51.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -       16.8217   57.0000  -90.0000 53

  7 omega  -86.00    1.00   1.0000    6.8300
omega____ theta____ kappa____ phi______ frames
    -      -17.2514  -57.0000  120.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0046526000
_diffrn_orient_matrix_UB_12      0.0375590000
_diffrn_orient_matrix_UB_13      0.0295590000
_diffrn_orient_matrix_UB_21      -0.0640023000
_diffrn_orient_matrix_UB_22      -0.0088579000
_diffrn_orient_matrix_UB_23      0.0002036000
_diffrn_orient_matrix_UB_31      0.0274307000
_diffrn_orient_matrix_UB_32      -0.0269809000
_diffrn_orient_matrix_UB_33      0.0410332000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25710
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.625
_diffrn_reflns_theta_min         3.939
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0390P)^2^+1.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4101
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00962h2.cif
_cod_data_source_block           exp_4497
_cod_depositor_comments
'Adding full bibliography for 7704295--7704299.cif.'
_cod_original_cell_volume        2296.19(18)
_cod_database_code               7704298
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C20 H35 Rh1 P1 N2 Cl1 O1'
_chemical_oxdiff_usercomment     'Ceci Rh71'
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.59
_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:
 C16(H16A,H16B), C19(H19A,H19B), C17(H17A,H17B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              94641
_olex2_submission_special_instructions 'No special instructions were received'