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_1572837
_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         '0.5(C88 H74 O6 P4 Re2), 0.5(C7 H8)'
_chemical_formula_sum            'C47.5 H41 O3 P2 Re'
_chemical_formula_weight         907.94
_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   mixed
_audit_creation_date             2022-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                75.285(3)
_cell_angle_beta                 68.908(3)
_cell_angle_gamma                83.041(3)
_cell_formula_units_Z            4
_cell_length_a                   14.9819(6)
_cell_length_b                   14.9880(4)
_cell_length_c                   19.2809(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3904.8(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.953
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22474
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.053
_diffrn_reflns_theta_min         3.302
_exptl_absorpt_coefficient_mu    7.188
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         14375
_refine_ls_number_restraints     642
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0354P)^2^+1.7473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11913
_reflns_number_total             14375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05369a2.cif
_cod_data_source_block           cui51cu_173k_final
_cod_depositor_comments
'Adding full bibliography for 1572837--1572839.cif.'
_cod_original_formula_sum        'C47.50 H41 O3 P2 Re'
_cod_database_code               1572837
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.597
_shelx_estimated_absorpt_t_min   0.533
_olex2_refinement_description
;
1. Restrained distances
 C7A-C6A
 1.4 with sigma of 0.01
 C7S-C1S
 1.52 with sigma of 0.02
 C4A-C6A
 2.42 with sigma of 0.04
 C7A-C3A
 2.42 with sigma of 0.04
 C6A-C8A
 2.42 with sigma of 0.04
 C5A-C7A
 2.42 with sigma of 0.04
 C3A-C5A
 2.42 with sigma of 0.04
 C6S-C4S
 2.4 with sigma of 0.04
 C7S-C6S
 2.54 with sigma of 0.04
 C2S-C4S
 2.4 with sigma of 0.04
 C7S-C2S
 2.54 with sigma of 0.04
 C1S-C5S
 2.4 with sigma of 0.04
 C1S-C3S
 2.4 with sigma of 0.04
 C6SA-C7SA
 2.54 with sigma of 0.04
 C2SA-C7SA
 2.54 with sigma of 0.04
 C4SA-C6SA
 2.4 with sigma of 0.04
 C3SA-C1SA
 2.4 with sigma of 0.04
 C5SA-C3SA
 2.4 with sigma of 0.04
 C1SA-C5SA
 2.4 with sigma of 0.04
 C4B-C3B \\sim C4B-C5B \\sim C5B-C6B \\sim C6B-C7B \\sim C7B-C8B \\sim C8B-C3B
 with sigma of 0.02
 C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C7A-C6A \\sim C8A-C7A \\sim C8A-C3A
 with sigma of 0.02
 C1S-C2S \\sim C2S-C3S \\sim C4S-C3S \\sim C5S-C4S \\sim C5S-C6S \\sim C1S-C6S
 with sigma of 0.02
 C2SA-C1SA \\sim C3SA-C2SA \\sim C4SA-C3SA \\sim C5SA-C4SA \\sim C6SA-C5SA
\\sim C6SA-C1SA
 with sigma of 0.02
 C3B-C2B \\sim C3A-C2A
 with sigma of 0.02
 C8C-C6C \\sim C4-C6
 with sigma of 0.04
 C8C-C4C \\sim C4-C8
 with sigma of 0.04
 C7C-C5C \\sim C5-C7
 with sigma of 0.04
 C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C7-C6 \\sim C8-C7 \\sim C8-C3
 with sigma of 0.02
 C2-C4C \\sim C2-C8
 with sigma of 0.04
 C8C-C7C \\sim C4-C5
 with sigma of 0.02
 C3C-C8C \\sim C3-C4
 with sigma of 0.02
 C5C-C4C \\sim C7-C8
 with sigma of 0.02
 C3C-C4C \\sim C3-C8
 with sigma of 0.02
 C6C-C5C \\sim C6-C7
 with sigma of 0.02
 C2-C8C \\sim C2-C4
 with sigma of 0.04
 C3C-C7C \\sim C3-C5
 with sigma of 0.04
 C7C-C6C \\sim C5-C6
 with sigma of 0.02
 C2-C3C \\sim C2-C3
 with sigma of 0.02
 C8C-C3C \\sim C7C-C8C \\sim C6C-C7C \\sim C5C-C6C \\sim C4C-C5C \\sim C4C-C3C
 with sigma of 0.02
 C3C-C5C \\sim C3-C7
 with sigma of 0.04
 C6C-C4C \\sim C6-C8
 with sigma of 0.04
 C1A-C2B \\sim C1A-C2A
 with sigma of 0.02
2. Restrained planarity
 C3A, C4A, C5A, C6A, C7A, C8A
 with sigma of 0.02
 C3B, C8B, C7B, C6B, C5B, C4B
 with sigma of 0.02
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma of 0.02
 C1S, C2S, C3S, C4S, C5S, C6S, C7S
 with sigma of 0.02
 C1SA, C2SA, C3SA, C4SA, C5SA, C6SA, C7SA
 with sigma of 0.02
 C2, C3C, C8C, C7C, C6C, C5C
 with sigma of 0.02
 C2, C3, C4, C5, C6, C7, C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C7B)
\\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq,
Uanis(C5A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C2A) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C3B)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C4S)
\\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(C6S) \\sim Ueq, Uanis(C7S) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C5SA) \\sim Ueq, Uanis(C7SA) \\sim Ueq, Uanis(C1SA) \\sim Ueq,
Uanis(C2SA) \\sim Ueq, Uanis(C6SA) \\sim Ueq, Uanis(C3SA) \\sim Ueq,
Uanis(C4SA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6C) \\sim Ueq, Uanis(C5C)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 C3B, C8B, C7B, C6B, C5B, C4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3A, C4A, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C2B, C3B, C8B, C7B, C6B, C5B, C4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1S, C2S, C3S, C4S, C5S, C6S, C7S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1SA, C2SA, C3SA, C4SA, C5SA, C6SA, C7SA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3C, C8C, C7C, C6C, C5C, C4C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C2B(0.5) H2BA(0.5) H2BB(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) C3B(0.5)
 C3A(0.5) C8B(0.5) H8B(0.5) C4A(0.5) H4A(0.5) C7B(0.5) H7B(0.5) C5A(0.5)
 H5A(0.5) C6B(0.5) H6B(0.5) C6A(0.5) H6A(0.5) C5B(0.5) H5B(0.5) C7A(0.5)
 H7A(0.5) C4B(0.5) H4B(0.5) C8A(0.5) H8A(0.5) H2BE(0.765) H2BF(0.765)
 H2AC(0.235) H2AD(0.235) C3(0.235) C3C(0.765) C4(0.235) H4(0.235) C8C(0.765)
 H8C(0.765) C5(0.235) H5(0.235) C7C(0.765) H7C(0.765) C6(0.235) H6(0.235)
 C6C(0.765) H6C(0.765) C7(0.235) H7(0.235) C5C(0.765) H5C(0.765) C8(0.235)
 H8(0.235) C4C(0.765) H4C(0.765) C1S(0.6667) C2S(0.6667) H2S(0.6667)
 C3S(0.6667) H3S(0.6667) C4S(0.6667) H4S(0.6667) C5S(0.6667) H5S(0.6667)
 C6S(0.6667) H6S(0.6667) C7S(0.6667) H7SA(0.6667) H7SB(0.6667) H7SC(0.6667)
 C1SA(0.3333) C2SA(0.3333) H2SA(0.3333) C3SA(0.3333) H3SA(0.3333) C4SA(0.3333)
 H4SA(0.3333) C5SA(0.3333) H5SA(0.3333) C6SA(0.3333) H6SA(0.3333) C7SA(0.3333)
 H7SD(0.3333) H7SE(0.3333) H7SF(0.3333)
6.a Rotating group:
 O3A(H3AA,H3AB), O3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C2A(H2AA,H2AB), C2(H2BE,H2BF), C2(H2AC,H2AD)
6.c Aromatic/amide H refined with riding coordinates:
 C8B(H8B), C4A(H4A), C7B(H7B), C5A(H5A), C6B(H6B), C6A(H6A), C5B(H5B),
 C7A(H7A), C4B(H4B), C8A(H8A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A), C44A(H44A),
 C45A(H45A), C46A(H46A), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A),
 C56A(H56A), C66A(H66A), C65A(H65A), C64A(H64A), C63A(H63A), C62A(H62A), C4(H4),
  C8C(H8C), C5(H5), C7C(H7C), C6(H6), C6C(H6C), C7(H7), C5C(H5C), C8(H8),
 C4C(H4C), C23(H23), C24(H24), C25(H25), C26(H26), C13(H13), C14(H14), C15(H15),
  C16(H16), C56(H56), C55(H55), C54(H54), C53(H53), C52(H52), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C36(H36), C35(H35), C34(H34), C33(H33),
  C32(H32), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C2S(H2S),
 C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C2SA(H2SA), C3SA(H3SA), C4SA(H4SA),
 C5SA(H5SA), C6SA(H6SA)
6.d Idealised Me refined as rotating group:
 C7S(H7SA,H7SB,H7SC), C7SA(H7SD,H7SE,H7SF)
;
_shelx_res_checksum              7838
_shelx_hkl_checksum              57033
_olex2_submission_special_instructions 'No special instructions were received'