Influence of substituents in aryl groups on the structure, thermal transitions and electrorheological properties of zinc bis(diarylphosphate) hybrid polymers
Dębowski, Maciej; Guńka, Piotr Aleksander; Żurawski, Konrad; Zybert, Magdalena; Modzelewska, Beata; Ostrowski, Andrzej; Zachara, Janusz; Florjańczyk, Zbigniew Jan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00492E

data_7709881
_publ_section_title
;
 Influence of substituents in aryl groups on the structure, thermal
 transitions and electrorheological properties of zinc
 bis(diarylphosphate) hybrid polymers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00492E
_journal_year                    2022
_chemical_formula_moiety         'C36 H36 O16 P2 Zn'
_chemical_formula_sum            'C36 H36 O16 P2 Zn'
_chemical_formula_weight         851.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                112.6738(18)
_cell_angle_beta                 95.5240(16)
_cell_angle_gamma                102.3836(19)
_cell_formula_units_Z            2
_cell_length_a                   8.8426(2)
_cell_length_b                   14.6002(3)
_cell_length_c                   17.1931(3)
_cell_measurement_reflns_used    25296
_cell_measurement_temperature    295
_cell_measurement_theta_max      31.0380
_cell_measurement_theta_min      3.4750
_cell_volume                     1960.67(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.0
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -97.00  -16.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  154.0000  -21.9666 81

  2 omega  -91.00    7.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  -77.0000  120.0000 98

  3 omega  -95.00  -15.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  152.0000  130.8926 80

  4 omega  -93.00   12.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  -77.0000 -120.0000 105

  5 omega  -94.00   -9.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  -57.0000    0.0000 85

  6 omega  -54.00   24.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -57.0000    0.0000 78

  7 omega  -23.00   66.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -19.0000   60.0000 89

  8 omega  -43.00   54.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -77.0000  -90.0000 97

  9 omega -109.00  -34.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560 -179.0000 -150.0000 75

 10 omega  -94.00   10.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  -57.0000 -180.0000 104

 11 omega -109.00  -34.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560 -179.0000   60.0000 75

 12 omega  -98.00   14.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  -77.0000  -30.0000 112

 13 omega  -56.00   47.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -38.0000   30.0000 103

 14 omega  -56.00   47.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -38.0000 -150.0000 103

 15 omega  -95.00  -14.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  152.0000   70.0280 81

 16 omega  -53.00   59.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560   77.0000  -60.0000 112

 17 omega  -49.00   54.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560   57.0000  120.0000 103

 18 omega   -9.00   94.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248   57.0000   90.0000 103

 19 omega   -4.00   62.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -99.0000 -150.0000 66

 20 omega   24.00   82.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248 -133.0000   31.9205 58

 21 omega  -97.00  -15.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  154.0000  -96.7092 82

 22 omega -100.00  -39.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6560  161.0000 -179.6264 61

 23 omega   -4.00   62.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -99.0000  120.0000 66

 24 omega   -9.00   94.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       20.1248   57.0000  150.0000 103
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0578386000
_diffrn_orient_matrix_UB_12      -0.0265604000
_diffrn_orient_matrix_UB_13      0.0015573000
_diffrn_orient_matrix_UB_21      0.0545642000
_diffrn_orient_matrix_UB_22      0.0357725000
_diffrn_orient_matrix_UB_23      -0.0093576000
_diffrn_orient_matrix_UB_31      0.0264320000
_diffrn_orient_matrix_UB_32      0.0318090000
_diffrn_orient_matrix_UB_33      0.0446213000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            116037
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        29.999
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plank
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         11434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0466P)^2^+0.8855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8906
_reflns_number_total             11434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00492e2.cif
_cod_data_source_block           ZnDECP_pg47
_cod_database_code               7709881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn P2 O10 C24 H16'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C8(H8A,H8B), C18(H18A,H18B), C28(H28A,H28B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              81345
_shelx_hkl_checksum              88077
_olex2_submission_special_instructions 'No special instructions were received'