Self-assembled supramolecular cages containing ruthenium(II) polypyridyl complexes
Jiajia Yang; Mohan Bhadbhade; William A. Donald; Hasti Iranmanesh; Evan G. Moore; Hong Yan; Jonathon E. Beves; Chem.Commun. 51 (2015) 4465–; doi:10.1039/C4cc10292D

data_7116645
_publ_section_title
;
 Self-assembled supramolecular cages containing ruthenium(II) polypyridyl
 complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              4465
_journal_paper_doi               10.1039/C4cc10292D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '1.25(F6 P), C62 H42 N10 Ru, C H3 N O2'
_chemical_formula_sum            'C63 H45 F7.5 N11 O2 P1.25 Ru'
_chemical_formula_weight         1270.38
_chemical_name_systematic        C63H45.7F9N11O4.2P1.5Ru
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-01-26 deposited with the CCDC.
2015-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.584(6)
_cell_length_b                   16.937(3)
_cell_length_c                   26.449(5)
_cell_measurement_temperature    100
_cell_volume                     13649(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            113586
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_min         1.376
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             5170
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Nitromethane'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0065(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         15544
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1253P)^2^+28.4767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14230
_reflns_number_total             15544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10292d2.cif
_cod_data_source_block           c2onc_a
_cod_original_formula_sum        'C63 H45 F7.50 N11 O2 P1.25 Ru'
_cod_database_code               7116645
_publcif_datablock.id            {6a5d77ff-043b-4737-a4a9-6c7a83058905}
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C58, C58'}
3. Restrained distances
 F3-F6 \\sim F3-F4 \\sim F3-F5 \\sim F3-F2 \\sim F6-F5 \\sim F6-F1 \\sim F6-F2
\\sim F4-F5 \\sim F4-F1 \\sim F1-F2
 with sigma of 0.04
 P1-F3 \\sim P1-F6 \\sim P1-F4 \\sim P1-F5 \\sim P1-F1 \\sim P1-F2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C58) = Uanis(C58')
5. Rigid body (RIGU) restrains
 P1, F3, F6, F4, F5, F1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C62'(0.65) H62'(0.65) C61'(0.65) H61'(0.65) C59(0.35) H59(0.35)
 C62(0.35) H62(0.35) C61(0.35) H61(0.35) C60(0.35) H60(0.35) C59'(0.65)
 H59'(0.65) C58(0.65) C60'(0.65) H60'(0.65) N10'(0.65) N10(0.35) C58'(0.35)
 P1(0.25) F1(0.25) F2(0.25) F3(0.25) F4(0.25) F5(0.25) F6(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C7(H7), C19(H19), C18(H18), C29(H29),
 C28(H28), C27(H27), C24(H24), C22(H22), C62'(H62'), C38(H38), C35(H35),
 C34(H34), C33(H33), C49(H49), C48(H48), C47(H47), C46(H46), C45(H45), C44(H44),
  C43(H43), C40(H40), C61'(H61'), C59(H59), C57(H57), C55(H55), C53(H53),
 C50(H50), C62(H62), C61(H61), C60(H60), C59'(H59'), C60'(H60'), C17(H17),
 C16(H16), C15(H15), C14(H14), C13(H13), C12(H12), C30(H30), C32(H32), C31(H31)
7.b Idealised Me refined as rotating group:
 C02F(H02A,H02B,H02C)
;
_shelx_res_checksum              61507
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'