Flexibility-driven 1D-structural preference in a bis-terpyridine-Fe(ii)-metallo-supramolecular polymer possessing potential tricolor electrochromism
Tripathi, Shivani; Halder, Sayan; Prusti, Banchhanidhi; Chakraborty, Chanchal; Chakravarty, Manab; Polymer Chemistry 14 (2023) 1359–1368; doi:10.1039/D2PY01557A

data_1568502
_publ_section_title
;
 Flexibility-driven 1D-structural preference in a
 bis-terpyridine-Fe(ii)-metallo-supramolecular polymer possessing
 potential tricolor electrochromism
;
_journal_issue                   12
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1359
_journal_page_last               1368
_journal_paper_doi               10.1039/D2PY01557A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C49 H43 N7'
_chemical_formula_sum            'C49 H43 N7'
_chemical_formula_weight         729.90
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-12-10 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.802(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5275(2)
_cell_length_b                   8.93710(10)
_cell_length_c                   31.1191(5)
_cell_measurement_reflns_used    13058
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.4540
_cell_measurement_theta_min      4.7550
_cell_volume                     3939.87(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     27.00  89.00   0.50    2.01    --    0.00  77.00-150.00  124
  2  \w    -17.00  64.00   0.50    2.01    --    0.00  37.00  90.00  162
  3  \w     -5.00  21.00   0.50    2.01    --    0.00  37.00 -60.00   52
  4  \w    -27.00  22.00   0.50    2.01    --    0.00  77.00-150.00   98
  5  \w     39.00  65.00   0.50    2.01    --    0.00  37.00 -60.00   52
  6  \w     88.00 140.00   0.50    8.03    --  107.20 -82.00  60.00  104
  7  \w     30.00  56.00   0.50    8.03    --  107.20 -61.00 120.00   52
  8  \w     83.00 155.00   0.50    8.03    --  107.20  61.00 -90.00  144
  9  \w     88.00 151.00   0.50    8.03    --  107.20  30.00  60.00  126
 10  \w     91.00 117.00   0.50    8.03    --  107.20 -82.00-180.00   52
 11  \w    159.00 184.00   0.50    8.03    --  107.20  30.00  60.00   50
 12  \w     24.00  83.00   0.50    8.03    --  107.20 -82.00  60.00  118
 13  \w     18.00 121.00   0.50    8.03    --  107.20 -61.00-180.00  206
 14  \w     83.00 116.00   0.50    8.03    --  107.20  15.00 -90.00   66
 15  \w     41.00  79.00   0.50    8.03    --  107.20 -82.00-180.00   76
 16  \w    140.00 166.00   0.50    8.03    --  107.20  15.00 -90.00   52
 17  \w     20.00 135.00   0.50    8.03    --  107.20 -82.00 120.00  230
 18  \w     84.00 109.00   0.50    8.03    --  107.20 -82.00  90.00   50
 19  \w     18.00  95.00   0.50    8.03    --  107.20 -15.00 -90.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0196003000
_diffrn_orient_matrix_UB_12      -0.1695073000
_diffrn_orient_matrix_UB_13      0.0037120000
_diffrn_orient_matrix_UB_21      -0.1018668000
_diffrn_orient_matrix_UB_22      -0.0277422000
_diffrn_orient_matrix_UB_23      0.0047607000
_diffrn_orient_matrix_UB_31      -0.0324241000
_diffrn_orient_matrix_UB_32      -0.0152078000
_diffrn_orient_matrix_UB_33      -0.0504193000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            27066
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.931
_diffrn_reflns_theta_min         4.776
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull yellowish colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0619P)^2^+1.0895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7160
_reflns_number_total             8357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01557a2.cif
_cod_data_source_block           exp_1253_st-dipyl
_cod_depositor_comments          'Adding full bibliography for 1568502.cif.'
_cod_database_code               1568502
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00T(H00B,H00C), C00U(H00E,H00F), C00Z(H00G,H00H), C014(H01A,H01B), C018(H01C,
 H01D), C01F(H01J,H01K)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00A), C00D(H00D), C00I(H00I), C00K(H00K), C00L(H00L),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C010(H010), C012(H012), C013(H013), C015(H015), C016(H016), C017(H017),
 C019(H019), C01A(H01E), C01B(H01F), C01C(H01G), C01D(H01H), C01E(H01I),
 C01G(H01L), C01H(H01M), C01I(H01N), C01K(H01R)
2.c Idealised Me refined as rotating group:
 C01J(H01O,H01P,H01Q)
;
_shelx_res_checksum              2456
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.690
_oxdiff_exptl_absorpt_empirical_full_min 0.634