π-Metalated [1<sub>5</sub>]Paracyclophanes: Synthesis and Binding to Oxo-Anions via Anion-π Interactions.
Zeng, Hong; Liu, Peiren; Feng, Guoqin; Huang, Feihe; Journal of the American Chemical Society 141 (2019) 16501–16511; doi:10.1021/jacs.9b09582

data_4127656
_publ_section_title
;
 \p-Metalated [1<sub>5</sub>]Paracyclophanes: Synthesis and Binding to
 Oxo-Anions via Anion-\p Interactions.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16501
_journal_page_last               16511
_journal_paper_doi               10.1021/jacs.9b09582
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C41 H36 Ru, 2(C F3 O3 S)'
_chemical_formula_sum            'C43 H36 F6 O6 Ru S2'
_chemical_formula_weight         927.91
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.338(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8009(7)
_cell_length_b                   41.745(3)
_cell_length_c                   14.4534(12)
_cell_measurement_reflns_used    5087
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.12
_cell_measurement_theta_min      2.812
_cell_volume                     4705.4(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.12
_diffrn_reflns_av_unetI/netI     0.1189
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_number            8863
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.509
_diffrn_reflns_theta_min         2.815
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.712
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 81327 reflections, Rint = 0.1719
 (24678 with I > 3sig(I), Rint = 0.1248)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.686
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.1218
_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^)+(0.0700P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2610
_refine_ls_wR_factor_ref         0.2863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5260
_reflns_number_total             8863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09582_si_002.cif
_cod_data_source_block           wmj18183
_cod_original_cell_volume        4705.5(7)
_cod_database_code               4127656
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.773
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.097) H2(0.099) H3(0.099) H4(0.106) H5(0.102) H6(0.102)
 H7(0.079) H8(0.091) H10(0.085) H11(0.085) H13A(0.097) H13B(0.097) H15(0.111)
 H16(0.127) H18(0.126) H19(0.122) H20A(0.14) H20B(0.14) H22(0.158) H23(0.129)
 H25(0.135) H26(0.155) H27A(0.115) H27B(0.115) H29(0.11) H30(0.095) H32(0.089)
 H33(0.101) H34A(0.099) H34B(0.099) H36(0.087) H37(0.086) H39(0.091) H40(0.093)
 H41A(0.092) H41B(0.092)
 Fixed X: H1(1.158766) H2(0.879374) H3(0.652863) H4(0.695476) H5(0.971552)
 H6(1.212956) H7(1.177825) H8(1.188057) H10(0.661618) H11(0.659329)
 H13A(0.795433) H13B(0.998601) H15(0.684282) H16(0.724164) H18(1.225935)
 H19(1.193063) H20A(0.903814) H20B(1.107996) H22(0.762423) H23(0.756479)
 H25(1.258897) H26(1.256203) H27A(0.91734) H27B(1.121337) H29(0.725933)
 H30(0.695396) H32(1.209173) H33(1.236809) H34A(0.818009) H34B(1.022028)
 H36(0.663964) H37(0.67452) H39(1.189335) H40(1.182345) H41A(1.038351)
 H41B(0.832954)
 Fixed Y: H1(0.281814) H2(0.265922) H3(0.298185) H4(0.347601) H5(0.366333)
 H6(0.33536) H7(0.376408) H8(0.324946) H10(0.322301) H11(0.374219)
 H13A(0.418747) H13B(0.417623) H15(0.444592) H16(0.480077) H18(0.477538)
 H19(0.440667) H20A(0.522522) H20B(0.519021) H22(0.497831) H23(0.467581)
 H25(0.453664) H26(0.48054) H27A(0.445494) H27B(0.441359) H29(0.402502)
 H30(0.347643) H32(0.338236) H33(0.391601) H34A(0.294385) H34B(0.289846)
 H36(0.29903) H37(0.293447) H39(0.287664) H40(0.297032) H41A(0.274042)
 H41B(0.272416)
 Fixed Z: H1(0.696754) H2(0.667046) H3(0.703065) H4(0.773859) H5(0.801131)
 H6(0.750624) H7(0.556415) H8(0.487006) H10(0.481926) H11(0.543739)
 H13A(0.620885) H13B(0.641603) H15(0.478659) H16(0.359668) H18(0.402838)
 H19(0.527401) H20A(0.293863) H20B(0.305291) H22(0.161998) H23(0.032388)
 H25(0.062666) H26(0.20181) H27A(-0.102014) H27B(-0.090504) H29(-0.040854) H30(-
 0.008083) H32(0.00687) H33(-0.032991) H34A(0.003488) H34B(0.006313)
 H36(0.149881) H37(0.312876) H39(0.310687) H40(0.153845) H41A(0.451157)
 H41B(0.448412)
;
_shelx_res_checksum              30432
_shelx_hkl_checksum              56036
_shelx_fab_checksum              97964
_olex2_submission_special_instructions 'No special instructions were received'