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_7704297
_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         'C21 H35 F3 N2 O4 P Rh S'
_chemical_formula_sum            'C21 H35 F3 N2 O4 P Rh S'
_chemical_formula_weight         602.45
_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     dual
_audit_creation_date             2020-04-24
_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                90
_cell_angle_beta                 99.9660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9238(5)
_cell_length_b                   12.2412(5)
_cell_length_c                   19.4780(8)
_cell_measurement_reflns_used    9117
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.33
_cell_volume                     2565.30(19)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         1.973
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0544 after correction.
The Ratio of minimum to maximum transmission is 0.8342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0208P)^2^+2.7895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4372
_reflns_number_total             5264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00962h2.cif
_cod_data_source_block           cmg276_0m
_cod_depositor_comments
'Adding full bibliography for 7704295--7704299.cif.'
_cod_database_code               7704297
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.725
_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. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Fixed Sof: C18(0.6) H18A(0.6) H18B(0.6) C18A(0.4) H18C(0.4) H18D(0.4)
 C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C21(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
 C20A(0.45) H20A(0.45) H20B(0.45) C20(0.55) H20C(0.55) H20D(0.55)
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C8(H8A,H8B), C18(H18A,H18B), C18A(H18C,H18D), C20A(H20A,H20B),
  C20(H20C,H20D)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C),
 C19A(H19D,H19E,H19F), C21A(H21A,H21B,H21C), C21(H21D,H21E,H21F)
;
_shelx_res_checksum              79995
_olex2_submission_special_instructions 'No special instructions were received'