A novel strategy to construct Janus metallamacrocycles with both a Ru‒arene face and an imidazolium face
Li, Ji; Zhang, Peipei; Xu, Yan; Su, Zhi; Qian, Yong; Li, Shunli; Yu, Tao; Sadler, Peter J.; Liu, Hong-Ke; Dalton Transactions  (2017) –; doi:10.1039/C7DT03374E

data_7044769
_publ_section_title
;
 A novel strategy to construct Janus metallamacrocycles with both a
 Ru--arene face and an imidazolium face
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03374E
_journal_year                    2017
_chemical_formula_moiety         'C47 H60 Cl N8 Ru, Cl, 2.0(Cl), 11.0(H2O)'
_chemical_formula_sum            'C47 H82 Cl4 N8 O11 Ru'
_chemical_formula_weight         1178.07
_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   mixed
_audit_creation_date             2017-10-10
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2017-10-17 deposited with the CCDC.
2017-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.956(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.568(5)
_cell_length_b                   31.904(5)
_cell_length_c                   14.478(5)
_cell_measurement_reflns_used    5628
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.8
_cell_volume                     5763(3)
_computing_data_collection       'Bruker, 2000'
_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    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Apex II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.753
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      0.05
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.974
_exptl_transmission_factor_min   0.951
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10139
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0593P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5778
_reflns_number_total             10139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03374e2.cif
_cod_data_source_block           a01
_cod_database_code               7044769
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.950
_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. Restrained distances
 C40-C45 \\sim C40-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C45-C47 \\sim C45A-C47A
 with sigma of 0.02
 C40-C46 \\sim C40-C46A
 with sigma of 0.04
 C40-C47 \\sim C40-C47A
 with sigma of 0.04
 C46-C47 \\sim C46A-C47A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C40, C45, C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C45A, C46A, C47A, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=
 Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(1)
 Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=FVAR(1)
5.a Riding coordinates:
 C4(H4A,H4B,H4C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C5(H5A,H5B,H5C),
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C),
 C46A(H46D,H46E,H46F)
5.b Ternary CH refined with riding coordinates:
 C45(H45), C45A(H45A)
5.c Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C23(H23A,H23B), C1(H1A,H1B), C16(H16A,H16B), C32(H32A,H32B)
5.d Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
5.e Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C10(H10), C9(H9), C35(H35), C21(H21), C6(H6), C20(H20),
 C36(H36), C42(H42), C41(H41), C14(H14), C39(H39), C17(H17), C15(H15), C18(H18)
5.f Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C47A(H47D,H47E,H47F)
;
_shelx_res_checksum              49600
_shelx_fab_checksum              9829
_olex2_submission_special_instructions 'No special instructions were received'