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_7709879
_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         'C28 H28 O12 P2 Zn'
_chemical_formula_sum            'C28 H28 O12 P2 Zn'
_chemical_formula_weight         683.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 99.8559(12)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   48.8533(7)
_cell_length_b                   9.85217(10)
_cell_length_c                   25.1339(3)
_cell_measurement_reflns_used    36378
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      32.4670
_cell_measurement_theta_min      3.7320
_cell_volume                     11918.7(3)
_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    'ShelXS n/a (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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    -84.00  -3.00   0.25   60.00    --  -19.49 -57.00 -30.00  324
  2  \w    -41.00  -8.00   0.25   60.00    --  -19.49  38.00-180.00  132
  3  \w    -23.00  44.50   0.25   60.00    --  -19.49  57.00 -90.00  270
  4  \w     29.00  62.00   0.25   60.00    --   19.96 -99.00-150.00  132
  5  \w      4.00  40.00   0.25   60.00    --   19.96  38.00 120.00  144
  6  \w      6.00  46.50   0.25   60.00    --   19.96 -99.00 -90.00  162
  7  \w    -38.00  -3.00   0.25   60.00    --  -19.49  38.00 -90.00  140
  8  \w     20.00  54.00   0.25   60.00    --  -19.49  57.00 120.00  136
  9  \w    -82.00 -36.00   0.25   60.00    --  -19.49-179.00  90.00  184
 10  \w    -49.00  14.00   0.25   60.00    --  -19.49  57.00 120.00  252
 11  \w     37.00  62.00   0.25   60.00    --   19.96 -99.00 150.00  100
 12  \w     73.00  98.00   0.25   60.00    --   19.96  77.00   0.00  100
 13  \w    -13.00  23.00   0.25   60.00    --   19.96  77.00   0.00  144
;
_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      0.0123385000
_diffrn_orient_matrix_UB_12      0.0161425000
_diffrn_orient_matrix_UB_13      0.0181729000
_diffrn_orient_matrix_UB_21      -0.0066443000
_diffrn_orient_matrix_UB_22      -0.0167799000
_diffrn_orient_matrix_UB_23      0.0221129000
_diffrn_orient_matrix_UB_31      0.0045528000
_diffrn_orient_matrix_UB_32      -0.0681221000
_diffrn_orient_matrix_UB_33      -0.0011544000
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            76610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 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    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         17323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+6.5833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15143
_reflns_number_total             17323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00492e2.cif
_cod_data_source_block           ZnDMP_md180_kwz178_b
_cod_database_code               7709879
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn2 P4 C56 H56 O24'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.746
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O24)=Sof(C57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(C61)=
 Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=1-FVAR(1)
 Sof(O25)=Sof(C50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(C54)=
 Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27),
  C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40),
 C41(H41), C44(H44), C45(H45), C47(H47), C48(H48), C51(H51), C52(H52), C54(H54),
  C55(H55), C58(H58), C59(H59), C61(H61), C62(H62)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              26818
_shelx_hkl_checksum              85293
_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 4.095
_oxdiff_exptl_absorpt_empirical_full_min 0.748