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_7043716
_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
'2(C40 H45 N7 O4 Zn), 1.68(H2 O), 4(Cl O4), 3.33(H2 O)'
_chemical_formula_sum            'C80 H100 Cl4 N14 O29 Zn2'
_chemical_formula_weight         1994.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-07-15 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.561(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.714(5)
_cell_length_b                   12.905(5)
_cell_length_c                   20.081(5)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.59
_cell_volume                     4597(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.296
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1205P)^2^+0.5749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5988
_reflns_number_total             8571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01364g2.cif
_cod_data_source_block           MC_ZnII_L1
_cod_database_code               7043716
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(O2)=Sof(O4AA)=1-FVAR(1)
 Sof(O0AA)=Sof(O2AA)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N2(H), N1(HB), N3(HK)
3.b Secondary CH2 refined with riding coordinates:
 C29(HF,HG), C5(HI,HJ), C0AA(HP,HQ), C30(HS,HT), C33(HU,HV), C43(HX,HY),
 C1(H1AA,H2AA), C18(H5AA,H6AA), C4(H9AA,H0BA), C37(H5BA,H6BA)
3.c Aromatic/amide H refined with riding coordinates:
 N7(HA), C10(HC), C11(HD), C7(HE), C8(HH), C19(HL), C13(HM), N8(HN), C16(HO),
 C22(HR), C20(HW), C14(HZ), C35(H0AA), C28(H3AA), C25(H4AA), C17(H7AA),
 C27(H8AA), C38(H1BA), C40(H2BA), C26(H3BA), C21(H4BA), C39(H7BA)
;
_shelx_res_checksum              42352
_olex2_submission_special_instructions 'No special instructions were received'