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_7704299
_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         'C22 H38 N3 O P Rh, C32 H12 B F24'
_chemical_formula_sum            'C54 H50 B F24 N3 O P Rh'
_chemical_formula_weight         1357.66
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-01 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                85.1790(10)
_cell_angle_beta                 67.2410(10)
_cell_angle_gamma                84.6680(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9981(4)
_cell_length_b                   14.4017(5)
_cell_length_c                   16.7912(5)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.756
_cell_measurement_theta_min      2.289
_cell_volume                     2881.99(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.833
_diffrn_reflns_theta_min         2.146
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.171
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         12323
_refine_ls_number_restraints     843
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0644P)^2^+5.3904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9115
_reflns_number_total             12323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00962h2.cif
_cod_data_source_block           cmg183_0m
_cod_depositor_comments
'Adding full bibliography for 7704295--7704299.cif.'
_cod_database_code               7704299
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.843
_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. Rigid body (RIGU) restrains
 F23, F24, F22, C37, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F23A, F24A, F22A, C37, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F11, F12, F10, C29, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F11A, F10A, F12A, C29, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: F16(0.5) F17(0.5) F18(0.5) F16A(0.5) F17A(0.5) F18A(0.5) F22(0.33)
 F23(0.27) F24(0.4) F22A(0.67) F24A(0.6) F23A(0.73) F13(0.5) F14(0.5) F15(0.5)
 F13A(0.5) F14A(0.5) F15A(0.5) F10(0.5) F11(0.65) F12(0.5) F10A(0.5) F11A(0.35)
 F12A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C24(H24), C26(H26), C28(H28), C32(H32), C34(H34),
 C36(H36), C40(H40), C42(H42), C44(H44), C48(H48), C50(H50), C52(H52)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              4442
_olex2_submission_special_instructions 'No special instructions were received'