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_7043715
_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_absolute_configuration
;
The Model has Chirality at N2 centre is R 
The Model has Chirality at N4 centre is S 
;
_chemical_formula_moiety
'C40 H47 N7 Ni O5, 2(Cl O4), 2(C H3 O H), H2 O'
_chemical_formula_sum            'C42 H57 Cl2 N7 Ni O16'
_chemical_formula_weight         1045.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-07-15 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4733(8)
_cell_length_b                   18.3502(10)
_cell_length_c                   19.0508(11)
_cell_measurement_reflns_used    3846
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.22
_cell_measurement_theta_min      2.16
_cell_volume                     4710.1(5)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER APEX 2'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'Bruker SXHELXTL'
_computing_publication_material  'Bruker SXHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.539
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.539
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37485
_diffrn_reflns_point_group_measured_fraction_full 0.527
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         20.725
_diffrn_reflns_theta_min         1.541
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 1353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         4883
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+10.7435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2168
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.512
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3823
_reflns_number_total             4883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01364g2.cif
_cod_data_source_block           MC_NiII_L1
_cod_database_code               7043715
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4
_shelx_res_checksum              36314