Syntheses of metallo-pseudorotaxanes, rotaxane and post-synthetically functionalized rotaxane: a comprehensive spectroscopic study and dynamic properties
Ghosh, Pradyut; Santra, Saikat; Bej, Somnath; Nandi, Mandira; Mondal, Partha; Dalton Trans.  (2017) –; doi:10.1039/C7DT01364G

data_7043717
_publ_section_title
;
 Syntheses of metallo-pseudorotaxanes, rotaxane and post-synthetically
 functionalized rotaxane: a comprehensive spectroscopic study and dynamic
 properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01364G
_journal_year                    2017
_chemical_formula_moiety         'C48 H59 Cu N9 O6, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C48 H63 Cl2 Cu N9 O16'
_chemical_formula_weight         1156.51
_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   mixed
_audit_creation_date             2017-07-13
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.07.04 svn.r3433 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2017-07-15 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                95.793(3)
_cell_angle_beta                 100.492(3)
_cell_angle_gamma                100.063(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4266(13)
_cell_length_b                   13.2646(15)
_cell_length_c                   18.043(2)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.32
_cell_volume                     2622.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'bruker apex-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27801
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.481
_diffrn_reflns_theta_min         1.574
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10602
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.3153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7008
_reflns_number_total             10602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01364g2.cif
_cod_data_source_block           MC_CuII_L3
_cod_original_cell_volume        2622.6(5)
_cod_database_code               7043717
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H14D-O5_$1
 1 with sigma of 0.1
 H14C-O10
 1 with sigma of 0.1
 Cl1-O8A \\sim Cl1A-O8B
 with sigma of 0.02
 Cl1-O6A \\sim Cl1A-O6B
 with sigma of 0.02
 Cl1-O10A \\sim Cl1A-O10B
 with sigma of 0.02
 Cl1-O12A \\sim Cl1A-O12B
 with sigma of 0.02
 O8A-O6A \\sim O8B-O6B
 with sigma of 0.04
 O8A-O10A \\sim O8B-O10B
 with sigma of 0.04
 O8A-O12A \\sim O8B-O12B
 with sigma of 0.04
 O6A-O10A \\sim O6B-O10B
 with sigma of 0.04
 O6A-O12A \\sim O6B-O12B
 with sigma of 0.04
 O10A-O12A \\sim O10B-O12B
 with sigma of 0.04
 C34-C35 \\sim C34-C35A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C34-C36 \\sim C34-C36A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C34, C35A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10B, Cl1A, O8B, O6B, O12B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl1A)=Sof(O8B)=Sof(O6B)=Sof(O10B)=Sof(O12B)=1-FVAR(1)
 Sof(Cl1)=Sof(O8A)=Sof(O6A)=Sof(O10A)=Sof(O12A)=FVAR(1)
 Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(2)
6.a Free rotating group:
 O14(H14C,H14D), O1B(H1BA,H1BB)
6.b Ternary CH refined with riding coordinates:
 N6(H6), N7(H7), N5(H5)
6.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C5(H5A,H5B), C16(H16A,H16B), C24(H24A,H24B), C4(H4A,H4B),
 C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C11(H11A,H11B), C14(H14A,H14B),
  C34(H34A,H34B), C34(H34C,H34D), C44(H44A,H44B), C35(H35A,H35B), C43(H43A,
 H43B), C35A(H35C,H35D)
6.d Aromatic/amide H refined with riding coordinates:
 C41(H41), C22(H22), C8(H8), C18(H18), C7(H7A), C19(H19), C26(H26), C21(H21),
 C10(H10), C27(H27), C1(H1), C2(H2), C38(H38), C30(H30), C29(H29), C39(H39),
 C32(H32), N2(H2A), N1(H1A), N3(H3), N4(H4), C47(H47)
6.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C1A(H1AA,H1AB,H1AC), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              33686
_olex2_submission_special_instructions 'No special instructions were received'