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_7709880
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H16 N4 O16 P2 Zn'
_chemical_formula_sum            'C24 H16 N4 O16 P2 Zn'
_chemical_formula_weight         743.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.54290(10)
_cell_length_b                   12.0207(2)
_cell_length_c                   30.3806(5)
_cell_measurement_reflns_used    25464
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      37.3640
_cell_measurement_theta_min      3.7820
_cell_volume                     2754.64(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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   -105.00  -2.00   1.00   36.00    --  -31.39 -57.00 -60.00  103
  2  \w   -102.00   2.00   1.00   36.00    --  -31.39 -77.00-120.00  104
  3  \w   -108.00  10.00   1.00   36.00    --  -31.39 -19.00  60.00  118
  4  \w    -60.00  42.00   1.00   36.00    --  -31.39  57.00-180.00  102
  5  \w    -50.00  45.00   1.00   36.00    --  -31.39  38.00  90.00   95
  6  \w   -110.00   2.00   1.00   36.00    --  -31.39 -77.00  60.00  112
  7  \w     -4.00  74.00   1.00   36.00    --   32.02 -99.00   0.00   78
  8  \w     38.00  96.00   1.00   36.00    --   32.02-137.00-177.00   58
  9  \w     56.00 122.00   1.00   36.00    --   32.02 179.00   0.00   66
 10  \w     -2.00 110.00   1.00   36.00    --   32.02  77.00-180.00  112
 11  \w    -50.00  45.00   1.00   36.00    --  -31.39  38.00-120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0527565000
_diffrn_orient_matrix_UB_12      0.0038586000
_diffrn_orient_matrix_UB_13      -0.0192543000
_diffrn_orient_matrix_UB_21      -0.0766630000
_diffrn_orient_matrix_UB_22      0.0076565000
_diffrn_orient_matrix_UB_23      0.0132011000
_diffrn_orient_matrix_UB_31      0.0135423000
_diffrn_orient_matrix_UB_32      0.0583700000
_diffrn_orient_matrix_UB_33      -0.0004616000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50852
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.793
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.993
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_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     425
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1848P)^2^+10.2526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2303
_refine_ls_wR_factor_ref         0.2320
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5297
_reflns_number_total             5436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00492e2.cif
_cod_data_source_block           ZnDNP_pg33_0-5maskssmart
_cod_database_code               7709880
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn P2 O16 N4 C24 H16'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(3)
 0.50(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(N4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24)
;
_shelx_res_checksum              46498
_shelx_hkl_checksum              98485
_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 1.669
_oxdiff_exptl_absorpt_empirical_full_min 0.609