Rotaxanes Derived from Dimetallic Polyynediyl Complexes: Extended Axles and Expanded Macrocycles
Baranová, Zuzana; Amini, Hashem; Bhuvanesh, Nattamai; Gladysz, John A.; Organometallics 33 (2014) 6746–; doi:10.1021/om501026u

data_4084835
_publ_section_title
;
 Rotaxanes Derived from Dimetallic Polyynediyl Complexes: Extended Axles
 and Expanded Macrocycles
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6746
_journal_paper_doi               10.1021/om501026u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'C108 H84 F10 P4 Pt2, C46 H44 N2 O4, 2(C6 H6)'
_chemical_formula_sum            'C166 H140 F10 N2 O4 P4 Pt2'
_chemical_formula_weight         2930.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-10-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                99.477(7)
_cell_angle_beta                 104.268(7)
_cell_angle_gamma                90.432(7)
_cell_formula_units_Z            2
_cell_length_a                   13.214(9)
_cell_length_b                   21.955(16)
_cell_length_c                   24.747(18)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.666
_cell_measurement_theta_min      2.325
_cell_volume                     6854(8)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    APEX-II
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.714
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.714
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39715
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         1.592
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.4425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0980 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.5941.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1681
_refine_ls_number_reflns         17699
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+10.0917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11770
_reflns_number_total             17699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501026u_si_005.cif
_cod_data_source_block           rotxr
_cod_depositor_comments
'Adding full bibliography for 4084834--4084835.cif.'
_cod_database_code               4084835
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.472
_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. Uiso/Uaniso restraints and constraints
C12 \\sim Pt2 \\sim C19: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C20) = Uanis(C19) = Uanis(C24)
Uanis(C12) = Uanis(C11) = Uanis(Pt2)
3. Rigid body (RIGU) restrains
 Pt1, C13, C18, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C19M(H19A,H19B), C20M(H20A,H20B), C21M(H21A,H21B), C22M(H22A,H22B), C23M(H23A,
 H23B), C24M(H24A,H24B), C35M(H35A,H35B), C36M(H36A,H36B), C37M(H37A,H37B),
 C38M(H38D,H38E), C39M(H39A,H39B), C40M(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36),
 C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C47(H47), C48(H48), C50(H50),
  C51(H51), C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62),
 C64(H64), C65(H65), C68(H68), C69(H69), C71(H71), C72(H72), C75(H75), C76(H76),
  C78(H78), C79(H79), C82(H82), C83(H83), C85(H85), C86(H86), C89(H89),
 C90(H90), C92(H92), C93(H93), C96(H96), C97(H97), C99(H99), C100(H100),
 C103(H103), C104(H104), C106(H106), C107(H107), C2M(H2M), C3M(H3M), C6M(H6M),
 C7M(H7M), C10M(H10M), C11M(H11M), C14M(H14M), C15M(H15M), C17M(H17M),
 C18M(H18M), C26M(H26M), C27M(H27M), C30M(H30M), C31M(H31M), C32M(H32M),
 C34M(H34M), C42M(H42M), C43M(H43M), C45M(H45M), C46M(H46M), C1S(H1S), C2S(H2S),
  C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C20S(H20S), C21S(H21S), C22S(H22S),
 C23S(H23S), C24S(H24S), C25S(H25S)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C52(H52A,H52B,
 H52C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C73(H73A,H73B,H73C), C80(H80A,
 H80B,H80C), C87(H87A,H87B,H87C), C94(H94A,H94B,H94C), C101(H10A,H10B,H10C),
 C108(H10D,H10E,H10F)
;
_shelx_res_checksum              15317
_shelx_hkl_checksum              15436