Solid-state polymerization in a polyrotaxane coordination polymer via a [2+2] cycloaddition reaction
In-Hyeok Park; Raghavender Medishetty; Shim Sung Lee; Jagadese J. Vittal; Chem.Commun. 50 (2014) 6585–; doi:10.1039/C4CC02080D

data_7113978
_publ_section_title
;
 Solid-state polymerization in a polyrotaxane coordination polymer via a
 [2+2] cycloaddition reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              6585
_journal_paper_doi               10.1039/C4CC02080D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C34 H24 Cd N2 O6 S'
_chemical_formula_weight         701.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.950(19)
_cell_angle_beta                 87.333(18)
_cell_angle_gamma                82.947(18)
_cell_formula_units_Z            2
_cell_length_a                   7.4493(18)
_cell_length_b                   15.362(4)
_cell_length_c                   15.558(4)
_cell_measurement_reflns_used    2075
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.68
_cell_volume                     1761.2(8)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1701
_diffrn_reflns_av_sigmaI/netI    0.2938
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19383
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.8633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;  
Total Potential Solvent Accessible Void Vol  356.0 Ang^3 (20.2%).
One pyridyl and olefin groups (N1-C7) were disordered. Two models 
were included in the ls refinements with ideal geometries to these
disordered groups. Only isotropic thermal parameters were fined (to
0.45(1)). Otherwise, the connectivity in the main structure is 
proven beyond any doubt. However, the solvent region was highly 
disordered as indicated by unreasonable thermal parameters and 
close contact indicated by CHECKCIF. This may be due 
to weakly diffracting nature as reflected from R(int) = 0.1701 and 
only 2804 reflections (> 2sigmaF^2) observed out of 6694 unique ref-
lections. When we attempted to construct model in the solvent 
region (DMA), the refinement was completed with R1 = 0.1096 and 
wR2 = 0.2747 with 393 parameters and 2799 observations. Further 
solvent region has problem as highlighted by the CIF. Moreover, due 
to very low data/parameter ratio, the data were squeezed. This 
model with the squeezed data has been found to be more acceptable.

;
_refine_diff_density_max         1.614
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6694
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1858
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.2023
_reflns_number_gt                2804
_reflns_number_total             6694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02080d2.cif
_cod_data_source_block           sqcd2
_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 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        1761.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113978