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_7704296
_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 N P Rh'
_chemical_formula_sum            'C20 H35 Cl N P Rh'
_chemical_formula_weight         458.82
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 105.066(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2786(5)
_cell_length_b                   13.4049(5)
_cell_length_c                   13.7401(5)
_cell_measurement_reflns_used    4553
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.0650
_cell_measurement_theta_min      4.1780
_cell_volume                     2183.79(15)
_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    'olex2.solve (Bourhis et al., 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 0.895
_diffrn_measurement_details
;
  1 omega  -21.00   89.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282   19.0000   30.0000 110

  2 omega  -54.00   39.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282  -37.0000   60.0000 93

  3 omega   35.00   91.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282  178.0000  -60.0000 56

  4 omega  -25.00   23.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -      -17.1016  -99.0000    0.0000 48

  5 omega  -25.00   23.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -      -17.1016  -99.0000   90.0000 48

  6 omega   -2.00   85.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282   57.0000  120.0000 87

  7 omega   -2.00   23.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282   57.0000 -120.0000 25

  8 omega  -52.00   35.00   1.0000   16.0700
omega____ theta____ kappa____ phi______ frames
    -       16.8282  -57.0000  -30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0174083000
_diffrn_orient_matrix_UB_12      -0.0009308000
_diffrn_orient_matrix_UB_13      -0.0453387000
_diffrn_orient_matrix_UB_21      0.0204826000
_diffrn_orient_matrix_UB_22      0.0495215000
_diffrn_orient_matrix_UB_23      0.0092597000
_diffrn_orient_matrix_UB_31      0.0534129000
_diffrn_orient_matrix_UB_32      -0.0186709000
_diffrn_orient_matrix_UB_33      0.0267786000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24195
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.438
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78425
_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            'metallic orangish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0498P)^2^+2.2058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3532
_reflns_number_total             5406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00962h2.cif
_cod_data_source_block           exp_4505
_cod_depositor_comments
'Adding full bibliography for 7704295--7704299.cif.'
_cod_original_cell_volume        2183.80(15)
_cod_database_code               7704296
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C20 H36 Rh1 P1 N1 Cl1'
_chemical_oxdiff_usercomment     'Ceci Rh77'
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.591
_reflns_odcompleteness_completeness 99.53
_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:
 C7(H7A,H7B), C16(H16A,H16B), C19(H19A,H19B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C10(H10A,H10B,H10C), C9(H9A,H9B,
 H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C18(H18A,
 H18B,H18C)
;
_shelx_res_checksum              39979
_olex2_submission_special_instructions 'No special instructions were received'