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_7709258
_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(C39 H39 Cl3 N4 O3 P Re), C4 H8 O, C H4 O'
_chemical_formula_sum            'C83 H90 Cl6 N8 O8 P2 Re2'
_chemical_formula_weight         1974.66
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-31
_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                 101.918(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0861(4)
_cell_length_b                   12.5731(3)
_cell_length_c                   26.9707(6)
_cell_measurement_reflns_used    13196
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      28.3260
_cell_measurement_theta_min      2.8300
_cell_volume                     4673.7(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.995
_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    -44.00  54.00   1.00   25.00    --  -19.81  38.00  30.00   98
  2  \w    -73.00  11.00   1.00   25.00    --  -19.81 -77.00-120.00   84
  3  \w   -109.00 -71.00   1.00   25.00    --  -19.81 179.00 -60.00   38
  4  \w     42.00  70.00   1.00   25.00    --  -19.81   0.00-180.00   28
  5  \w    -82.00  14.00   1.00   25.00    --  -19.81 -77.00 120.00   96
  6  \w    -83.00 -77.00   1.00   25.00    --  -19.81   0.00-180.00    6
;
_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      0.0033810000
_diffrn_orient_matrix_UB_12      -0.0042462000
_diffrn_orient_matrix_UB_13      -0.0258271000
_diffrn_orient_matrix_UB_21      0.0454500000
_diffrn_orient_matrix_UB_22      -0.0258444000
_diffrn_orient_matrix_UB_23      0.0073575000
_diffrn_orient_matrix_UB_31      -0.0238226000
_diffrn_orient_matrix_UB_32      -0.0499532000
_diffrn_orient_matrix_UB_33      -0.0016207000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36305
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.532
_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    1.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.683
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9589
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+38.3541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7794
_reflns_number_total             9589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03966k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7709258--7709259.cif.'
_cod_database_code               7709258
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C83 H90 Cl6 N8 O8 P2 Re2'
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.419
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9561(7)
 0.0439(7)
2. 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, All O(H) groups
3. Restrained distances
 O4-C40 = C43-O4
 1.45 with sigma of 0.01
 C40-C41 = C41-C42 = C42-C43
 1.52 with sigma of 0.01
 O4-C41 = C40-C42 = C41-C43 = C42-O4
 2.45 with sigma of 0.02
 O5-C44 \\sim O6-C45
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O5 \\sim C44 \\sim O6 \\sim C45: within 3A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 3A
O4 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 3A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 3A
5. Others
 Fixed Sof: O4(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) C43(0.5) H43A(0.5) H43B(0.5) O5(0.25) H5A(0.25)
 C44(0.25) H44A(0.25) H44B(0.25) H44C(0.25) O6(0.25) H6A(0.25) C45(0.25)
 H45A(0.25) H45B(0.25) H45C(0.25)
 Fixed X: H5A(0.42794) H6A(0.52206)
 Fixed Y: H5A(0.99766) H6A(0.86243)
 Fixed Z: H5A(0.98382) H6A(0.92845)
6.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
6.b 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), C20(H20), C21(H21),
  C24(H24), C26(H26), C33(H33), C35(H35)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              59435
_olex2_date_sample_data_collection 2011-09-07
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.869