Synthesis, structures and magnetic properties of isoreticular polyrotaxane-type two-dimensional coordination polymers
Park, In-Hyeok; Herng, Tun Seng; Ju, Huiyeong; Ding, Jun; Lee, Shim Sung; Vittal, Jagadese J.; RSC Adv. 7 (2017) 45582–; doi:10.1039/C7RA07637A

data_7229233
_publ_section_title
;
 Synthesis, structures and magnetic properties of isoreticular
 polyrotaxane-type two-dimensional coordination polymers
;
_journal_issue                   72
_journal_name_full               'RSC Adv.'
_journal_page_first              45582
_journal_paper_doi               10.1039/C7RA07637A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C40 H26 Co2 N2 O12 S2'
_chemical_formula_weight         908.61
_chemical_name_systematic        2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.056(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9968(12)
_cell_length_b                   22.1340(16)
_cell_length_c                   12.5998(9)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.26
_cell_volume                     4327.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40331
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.903
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
 PLATON shows solvent accessible void volume of 872.8 Ang^3 out of
 the cell volume, 4327.7(6) A^3 which is 20.17%. 
 Initially normal refinement was attempted which revealed that one of the 
 pyridyl groups of bpe (C1a -- C5a) was disordered. A common occupancy factor was 
 refined to 0.78(2). Further one DMA and 1.5 water molecules were found in the 
 voids. The DMA was disordered. Two orientations of the DMA molecules were 
 successfully resolved and a common occupancy factor was refined to 0.52(1). 
 Disordered water molecules were scattered in at least 4 different places in 
 the voids with different occupancies. The final agreement factors are: R1 = 
 0.0641 for 5972 (Fo>4sig(F0) and 0.0937 for all 8502 data. The wR2 = 0.1595 
 for 690 parameters and GooF = 1.095. Since the thermal parameters of the 
 atoms of the DMA molecule was not satisfactory, we have resorted to squeeze 
 the electrons of the voids using SQUEEZE program. The final agreement factors 
 were better and hence retained. 
 In the squeezed structure, the common occupancy factor of the disordered pyridyl 
 group was refined to 0.77(1). The final agreement factors are: R1 = 0.0602 for 
 6029 (Fo>4sig(F0) and 0.0829 for all 8502 data. The wR2 = 0.1540 for 560 
 parameters and GooF = 1.081.
;
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8502
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+10.0437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             8502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra07637a2.cif
_cod_data_source_block           xtl2r_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7229233
_shelx_estimated_absorpt_t_min   0.655
_shelx_estimated_absorpt_t_max   0.874
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              72417