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_7704295
_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 N2 O P Rh, C32 H12 B F24'
_chemical_formula_sum            'C52 H47 B F24 N2 O P Rh'
_chemical_formula_weight         1316.60
_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             2020-04-26
_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                 92.2640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2707(5)
_cell_length_b                   36.6662(14)
_cell_length_c                   12.3316(5)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.30
_cell_volume                     5543.9(4)
_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      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  0.0348
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            160081
_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         26.458
_diffrn_reflns_theta_min         2.297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0538 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.9331.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.516
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         11392
_refine_ls_number_restraints     1047
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0286P)^2^+15.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10326
_reflns_number_total             11392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00962h2.cif
_cod_data_source_block           cmg278xmonop21n_0m
_cod_depositor_comments
'Adding full bibliography for 7704295--7704299.cif.'
_cod_database_code               7704295
_shelx_shelxl_version_number     2017/1
_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
 C39A, C44A, F22A, F24A, F23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, F11A, F12A, F10A, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, F8A, F9A, F7A, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C42, C41, C40, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37A, C42A, C41A, C40A, C39A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51A, F15A, F13A, F14A, C49A
 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
3. Others
 Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=
 Sof(C50A)=Sof(H50A)=1-FVAR(1)
 Sof(C45)=Sof(C46)=Sof(H46)=Sof(C50)=Sof(H50)=Sof(C47)=Sof(C48)=Sof(H48)=
 Sof(C49)=FVAR(1)
 Sof(C52A)=Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(2)
 Sof(F16)=Sof(F18)=Sof(F17)=Sof(C52)=FVAR(2)
 Sof(F13A)=Sof(F15A)=1-FVAR(3)
 Sof(F15)=Sof(F13)=FVAR(3)
 Sof(F9)=1-FVAR(4)
 Sof(F9A)=FVAR(4)
 Sof(C37A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=
 Sof(C38A)=Sof(H38A)=1-FVAR(5)
 Sof(C37)=Sof(C42)=Sof(H42)=Sof(C41)=Sof(C40)=Sof(H40)=Sof(C39)=Sof(C38)=
 Sof(H38)=FVAR(5)
 Sof(C43)=Sof(F21)=Sof(F19)=Sof(F20)=1-FVAR(6)
 Sof(C43A)=Sof(F21A)=Sof(F20A)=Sof(F19A)=FVAR(6)
 Sof(F10A)=Sof(F12A)=1-FVAR(7)
 Sof(F10)=Sof(F12)=FVAR(7)
 Sof(F22A)=Sof(F24A)=Sof(F23A)=1-FVAR(8)
 Sof(F22)=Sof(F24)=Sof(F23)=FVAR(8)
 Sof(C44A)=1-FVAR(9)
 Sof(C44)=FVAR(9)
 Fixed Sof: F6(0.5) F4(0.5) F5(0.6) C28(0.7) F8A(0.63) F7A(0.75) F14(0.5)
 C51(0.55) C51A(0.45) F14A(0.5) C28A(0.3) F8(0.37) F7(0.25) F6A(0.5) F5A(0.4)
 F4A(0.5) F11(0.55) F11A(0.45)
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), C22(H22), C24(H24), C26(H26), C30(H30), C32(H32),
 C42(H42), C40(H40), C38(H38), C34(H34), C46(H46), C50(H50), C48(H48),
 C46A(H46A), C48A(H48A), C50A(H50A), C42A(H42A), C40A(H40A), C38A(H38A)
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)
;
_shelx_res_checksum              81460
_olex2_submission_special_instructions 'No special instructions were received'