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_4084834
_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, C42 H42 N2 O4, 0.5(C H Cl3)'
_chemical_formula_sum            'C150.5 H126.5 Cl1.5 F10 N2 O4 P4 Pt2'
_chemical_formula_weight         2784.26
_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             2013-12-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                92.508(3)
_cell_angle_beta                 96.172(3)
_cell_angle_gamma                107.174(3)
_cell_formula_units_Z            2
_cell_length_a                   12.601(3)
_cell_length_b                   20.408(4)
_cell_length_c                   26.978(5)
_cell_measurement_reflns_used    9144
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.302
_cell_measurement_theta_min      2.926
_cell_volume                     6569(2)
_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
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            186612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.362
_diffrn_reflns_theta_min         2.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1952 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.8644.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             2814
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1634
_refine_ls_number_reflns         32484
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0072P)^2^+9.4983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28628
_reflns_number_total             32484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501026u_si_005.cif
_cod_data_source_block           8229
_cod_depositor_comments
'Adding full bibliography for 4084834--4084835.cif.'
_cod_original_formula_sum        'C150.50 H126.50 Cl1.50 F10 N2 O4 P4 Pt2'
_cod_database_code               4084834
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.851
_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
 Cl3S-C1S \\sim Cl3T-C1T \\sim Cl1S-C1S \\sim Cl1T-C1T \\sim Cl2S-C1S \\sim
Cl2T-C1T
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1S \\sim Cl2S \\sim Cl3S \\sim Cl2T \\sim Cl1T \\sim Cl3T \\sim C1S \\sim
C1T: within 1.7A with sigma of 1.7 and sigma for terminal atoms of 3.4
4. Rigid body (RIGU) restrains
 Cl1S, Cl2S, Cl3S, Cl2T, Cl1T, Cl3T, C1S, C1T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1T)=Sof(H1T)=Sof(Cl2T)=Sof(Cl1T)=Sof(Cl3T)=0.5*(1-FVAR(2))
 Sof(C1S)=Sof(H1S)=Sof(Cl1S)=Sof(Cl2S)=Sof(Cl3S)=0.5*FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C1T(H1T)
6.b Secondary CH2 refined with riding coordinates:
 C19M(H19A,H19B), C20M(H20A,H20B), C21M(H21A,H21B), C22M(H22A,H22B), C23M(H23A,
 H23B), C24M(H24A,H24B), C31M(H31A,H31B), C32M(H32D,H32E), C33M(H33A,H33B),
 C34M(H34A,H34B), C35M(H35A,H35B), C36M(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C27(H27), C28(H28), C30(H30),
 C31(H31), C34(H34), C35(H35), C37(H37), C38(H38), C41(H41), C42(H42), C44(H44),
  C45(H45), C48(H48), C49(H49), C51(H51), C52(H52), C55(H55), C56(H56),
 C58(H58), C59(H59), 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), C28M(H28M), C30M(H30M), C38M(H38M),
 C39M(H39M), C41M(H41M), C42M(H42M)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C46(H46A,H46B,
 H46C), C53(H53A,H53B,H53C), C60(H60A,H60B,H60C), 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              22889
_shelx_hkl_checksum              63298