The reaction of rhenium nitrosyl with a sterically hindered NHC-carbene.
Grieco, G.; Blacque, O.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1521–1526; doi:10.1039/d1dt03966k

data_7709259
_publ_section_title
;
 The reaction of rhenium nitrosyl with a sterically hindered NHC-carbene.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1521
_journal_page_last               1526
_journal_paper_doi               10.1039/d1dt03966k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         '2(C18 H15 Cl3 N2 O3 P Re), 3(C7 H8)'
_chemical_formula_sum            'C57 H54 Cl6 N4 O6 P2 Re2'
_chemical_formula_weight         1538.08
_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     dual
_audit_creation_date             2021-08-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0987(2)
_cell_length_b                   9.01830(10)
_cell_length_c                   30.4320(5)
_cell_measurement_reflns_used    16102
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      29.6470
_cell_measurement_theta_min      2.9270
_cell_volume                     3017.29(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -9.00 100.00   1.00   60.00    --   16.00   0.00   0.00  109
  2  \w    -18.00  86.00   1.00   60.00    --   16.00  77.00-180.00  104
  3  \w    -36.00  -9.00   1.00   60.00    --  -15.21 -44.00  15.00   27
  4  \w   -103.00 -68.00   1.00   60.00    --  -15.21 179.00 -60.00   35
  5  \w    -18.00  61.00   1.00   60.00    --  -15.21  38.00 -60.00   79
  6  \w     67.00 100.00   1.00   60.00    --   16.00   0.00  30.00   33
  7  \w    -69.00 -35.00   1.00   60.00    --   16.00   0.00  30.00   34
  8  \w    -37.00 -12.00   1.00   60.00    --  -15.21 -89.00 -10.00   25
  9  \w    -42.00  45.00   1.00   60.00    --  -15.21  38.00-120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0442778000
_diffrn_orient_matrix_UB_12      -0.0004988000
_diffrn_orient_matrix_UB_13      0.0147378000
_diffrn_orient_matrix_UB_21      -0.0392872000
_diffrn_orient_matrix_UB_22      -0.0426137000
_diffrn_orient_matrix_UB_23      -0.0154745000
_diffrn_orient_matrix_UB_31      0.0256297000
_diffrn_orient_matrix_UB_32      -0.0661083000
_diffrn_orient_matrix_UB_33      0.0098555000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            42433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.632
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       plate
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7462
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0190P)^2^+3.6959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6012
_reflns_number_total             7462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03966k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7709258--7709259.cif.'
_cod_database_code               7709259
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C57 H54 Cl6 N4 O6 P2'
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.506
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C32
 1.55 with sigma of 0.01
 C20-C19 = C20A-C19A
 1.54 with sigma of 0.01
 C23A-C22A = C24A-C23A = C25A-C24A = C25A-C20A = C21A-C20A = C22A-C21A
 1.39 with sigma of 0.01
 C25-C20 = C25-C24 = C24-C23 = C23-C22 = C22-C21 = C21-C20
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C19A
\\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A: within 3A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 3A
4. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C23A)=Sof(H23A)=Sof(C20A)=
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(1)
 Fixed Sof: C26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5)
 C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
5.a :
 C20(C21,C22,C23,C24,C25), C23A(C20A,C21A,C22A,C24A,C25A)
5.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C23A(H23A), C21A(H21A), C22A(H22A), C24A(H24A),
 C25A(H25A), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
5.d Fitted hexagon refined as free rotating group:
 C26(C27,C28,C29,C30,C31)
5.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
;
_shelx_res_checksum              31443
_olex2_date_sample_data_collection 2011-01-12
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.443
_oxdiff_exptl_absorpt_empirical_full_min 0.851