Exploring efficient and air-stable d<sup>2</sup> Re(v) alkylidyne catalysts: toward room temperature alkyne metathesis.
Cui, Mingxu; Huang, Jie; Tsang, Long Yiu; Sung, Herman H. Y.; Williams, Ian D.; Jia, Guochen; Chemical science 15 (2024) 18318–18326; doi:10.1039/d4sc05369a

data_1572839
_publ_section_title
;
 Exploring efficient and air-stable d<sup>2</sup> Re(v) alkylidyne
 catalysts: toward room temperature alkyne metathesis.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              18318
_journal_page_last               18326
_journal_paper_doi               10.1039/d4sc05369a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C46 H41 O2 P2 Re S'
_chemical_formula_sum            'C46 H41 O2 P2 Re S'
_chemical_formula_weight         905.99
_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     dual
_audit_creation_date             2023-10-04
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.487(3)
_cell_angle_beta                 78.475(3)
_cell_angle_gamma                62.411(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0053(5)
_cell_length_b                   11.4390(4)
_cell_length_c                   17.8263(6)
_cell_measurement_reflns_used    10194
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.5160
_cell_measurement_theta_min      2.5230
_cell_volume                     1948.62(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.948
_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   -116.00 -23.00   1.00    2.00    --  -41.26 -37.00 -90.00   93
  2  \w    -64.00  32.00   1.00    2.00    --  -41.26  57.00  60.00   96
  3  \w    -15.00  73.00   1.00    2.00    --   41.26 -73.00 156.00   88
  4  \w     72.00 146.00   1.00    3.00    --  107.01 178.00 -90.00   74
  5  \w    103.00 152.00   1.00    3.00    --  107.01  77.00  30.00   49
  6  \w    109.00 143.00   1.00    3.00    --  107.01  45.00 -90.00   34
  7  \w     41.00 109.00   1.00    3.00    --  107.01-111.00-120.00   68
  8  \w     57.00 109.00   1.00    3.00    --  107.01-111.00  30.00   52
  9  \w    101.00 169.00   1.00    3.00    --  107.01  73.00 -74.00   68
 10  \w     89.00 173.00   1.00    3.00    --  107.01  45.00   0.00   84
 11  \w     42.00 132.00   1.00    3.00    --  107.01 -61.00-150.00   90
 12  \w    119.00 178.00   1.00    3.00    --  107.01 111.00-120.00   59
 13  \w     38.00 127.00   1.00    3.00    --  107.01 -45.00 -30.00   89
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1065809000
_diffrn_orient_matrix_UB_12      -0.0576477000
_diffrn_orient_matrix_UB_13      0.0540284000
_diffrn_orient_matrix_UB_21      -0.0776811000
_diffrn_orient_matrix_UB_22      0.1295546000
_diffrn_orient_matrix_UB_23      0.0473068000
_diffrn_orient_matrix_UB_31      -0.0918436000
_diffrn_orient_matrix_UB_32      -0.0546682000
_diffrn_orient_matrix_UB_33      0.0512256000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11819
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.619
_diffrn_reflns_theta_min         2.530
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0159
_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^)+(0.0209P)^2^+0.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7377
_reflns_number_total             7585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05369a2.cif
_cod_data_source_block           hjie5cu_173k_auto
_cod_depositor_comments
'Adding full bibliography for 1572837--1572839.cif.'
_cod_database_code               1572839
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.514
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.261
_oxdiff_exptl_absorpt_empirical_full_min 0.850