A Macrocyclic Ruthenium Carbene for Size-Selective Alkene Metathesis.
Zhang, Yutong; Diver, Steven T.; Journal of the American Chemical Society 142 (2020) 3371–3374; doi:10.1021/jacs.0c00081

data_4134130
_publ_section_title
;
 A Macrocyclic Ruthenium Carbene for Size-Selective Alkene Metathesis.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3371
_journal_page_last               3374
_journal_paper_doi               10.1021/jacs.0c00081
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C72 H65 Cl2 N4 O3 Ru, 3(C H2 Cl2), B F4'
_chemical_formula_sum            'C75 H71 B Cl8 F4 N4 O3 Ru'
_chemical_formula_weight         1547.83
_chemical_name_systematic        C75H72BCl8F4N4O3Ru
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.8848(11)
_cell_length_b                   18.2115(8)
_cell_length_c                   28.4594(13)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      2.24
_cell_volume                     13934.1(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            202799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         1.431
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0974 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.9375. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             6352
_exptl_crystal_recrystallization_method 'grown in benzene/dichloromethane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1736
_refine_ls_number_reflns         28517
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0962P)^2^+48.6874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22509
_reflns_number_total             28517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00081_si_002.cif
_cod_data_source_block           gsb_061802
_cod_depositor_comments          'Adding full bibliography for 4134130.cif.'
_cod_database_code               4134130
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(5)
 0.50(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C101 \\sim C98 \\sim C97 \\sim C96 \\sim C95 \\sim C94 \\sim C99 \\sim C100
\\sim C105 \\sim C104 \\sim C103 \\sim C102: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Others
 Sof(H14I)=Sof(H14J)=Sof(Cl10)=1-FVAR(1)
 Sof(Cl9)=Sof(H14G)=Sof(H14H)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C80(H80)
5.b Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C44(H44A,H44B), C115(H11G,H11H), C150(H15A,H15B), C12(H12D,
 H12E), C116(H11I,H11J), C43(H43A,H43B), C85(H85A,H85B), C145(H14G,H14H),
 C145(H14I,H14J), C13(H13A,H13B), C148(H14K,H14L), C149(H14M,H14N), C146(H14O,
 H14P), C147(H14Q,H14R)
5.c Aromatic/amide H refined with riding coordinates:
 C50(H50), C3(H3), C76(H76), C107(H107), C73(H73), C77(H77), C78(H78), C1(H1),
 C138(H138), C114(H114), C61(H61), C127(H127), C122(H122), C56(H56), C41(H41),
 C126(H126), C72(H72), C144(H144), C19(H19), C6(H6), C4(H4), C66(H66),
 C135(H135), C25(H25), C113(H113), C48(H48), C63(H63), C54(H54), C128(H128),
 C134(H134), C120(H120), C42(H42), C75(H75), C91(H91), C5(H5), C17(H17),
 C35(H35), C95(H95), C96(H96), C97(H97), C62(H62), C23(H23), C55(H55), C89(H89),
  C30(H30), C133(H133), C102(H102), C103(H103), C104(H104), C24(H24), C31(H31),
 C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C99(C94,C95,C96,C97,C98), C101(C102,C103,C104,C105,C100)
5.e Idealised Me refined as rotating group:
 C10(H10D,H10E,H10F), C81(H81A,H81B,H81C), C9(H9A,H9B,H9C), C140(H14A,H14B,
 H14C), C112(H11A,H11B,H11C), C119(H11D,H11E,H11F), C71(H71A,H71B,H71C),
 C93(H93A,H93B,H93C), C109(H10A,H10B,H10C), C52(H52A,H52B,H52C), C21(H21A,H21B,
 H21C), C82(H82A,H82B,H82C), C124(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C143(H14D,H14E,H14F), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C37(H37A,H37B,
 H37C), C88(H88A,H88B,H88C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              15748
_shelx_hkl_checksum              10514
_olex2_submission_special_instructions 'No special instructions were received'