Preparation of Sulfonic Acid Functional Proton Conducting Phosphazenes by Covalent Protection
Celebi, Elif Busra; Hacıvelioğlu, Ferda; Polym. Chem.  (2017) –; doi:10.1039/C7PY00189D

data_1545750
_publ_section_title
;
 Preparation of Sulfonic Acid Functional Proton Conducting Phosphazenes by
 Covalent Protection
;
_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY00189D
_journal_year                    2017
_chemical_formula_moiety         'C48 H54 N3 O24 P3 S6'
_chemical_formula_sum            'C48 H54 N3 O24 P3 S6'
_chemical_formula_weight         1342.21
_chemical_melting_point          410
_chemical_name_systematic        Phosphazene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-24 deposited with the CCDC.
2017-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7219(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9225(2)
_cell_length_b                   13.0558(2)
_cell_length_c                   30.1455(5)
_cell_measurement_reflns_used    24539
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      29.4440
_cell_measurement_theta_min      2.0970
_cell_volume                     5819.84(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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   -106.00  74.00   1.00    8.00    --  -16.00   0.00-120.00  180
  2  \w    -76.00  20.00   1.00    8.00    --  -16.00 -72.00 150.00   96
  3  \w    -89.00 -74.00   1.00    8.00    --  -16.00   0.00-150.00   15
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185983000
_diffrn_orient_matrix_UB_12      0.0499281000
_diffrn_orient_matrix_UB_13      -0.0028632000
_diffrn_orient_matrix_UB_21      -0.0227285000
_diffrn_orient_matrix_UB_22      -0.0072771000
_diffrn_orient_matrix_UB_23      0.0189652000
_diffrn_orient_matrix_UB_31      0.0379221000
_diffrn_orient_matrix_UB_32      0.0201089000
_diffrn_orient_matrix_UB_33      0.0140119000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38617
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_preparation       'As described in the journal'
_exptl_crystal_recrystallization_method THF:EtOH(1:1)
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         13195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0800P)^2^+8.7300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11305
_reflns_number_total             13195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00189d1.cif
_cod_data_source_block           316-tz-1z
_cod_original_cell_volume        5819.85(16)
_cod_database_code               1545750
_chemical_oxdiff_formula         'C48 H36 N3 O24 P3 S6'
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All C(H,H,H,H,H,H) groups
2. Others
 Sof(O4B)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H8BD)=Sof(H8BE)=Sof(H8BF)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(2)
 Sof(O8B)=1-FVAR(3)
 Sof(O8)=FVAR(3)
 Sof(O7B)=1-FVAR(4)
 Sof(O7)=FVAR(4)
 Sof(O3B)=1-FVAR(5)
 Sof(O3)=FVAR(5)
 Sof(O6B)=1-FVAR(6)
 Sof(O6)=FVAR(6)
 Sof(O24B)=1-FVAR(7)
 Sof(O24)=FVAR(7)
 Sof(C47A)=Sof(H47C)=Sof(H47D)=1-FVAR(8)
 Sof(C47)=Sof(H47A)=Sof(H47B)=FVAR(8)
 Sof(O23)=1-FVAR(9)
 Sof(O23B)=FVAR(9)
 Sof(C48)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(10)
 Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(10)
 Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(11)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(11)
 Sof(C42B)=Sof(H42B)=Sof(C43B)=Sof(H43B)=Sof(C45B)=Sof(H45B)=Sof(C46B)=
 Sof(H46B)=1-FVAR(12)
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 FVAR(12)
 Sof(O22B)=1-FVAR(13)
 Sof(O22)=FVAR(13)
 Sof(O2A)=1-FVAR(14)
 Sof(O2)=FVAR(14)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C7B(H7BA,H7BB), C15(H15A,H15B), C15B(H15C,H15D), C23(H23A,H23B),
 C31(H31A,H31B), C39(H39A,H39B), C47(H47A,H47B), C47A(H47C,H47D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18), C19(H19), C21(H21), C22(H22), C26(H26), C27(H27), C29(H29), C30(H30),
  C34(H34), C35(H35), C37(H37), C38(H38), C42(H42), C42B(H42B), C43(H43),
 C43B(H43B), C45(H45), C45B(H45B), C46(H46), C46B(H46B)
3.c Idealised Me refined as rotating group:
 C8(H8AA,H8AB,H8AC), C8(H8BD,H8BE,H8BF), C16(H16A,H16B,H16C), C16(H16D,H16E,
 H16F), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C),
 C48A(H48A,H48B,H48C), C48(H48D,H48E,H48F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 316-331-1
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.702
_oxdiff_exptl_absorpt_empirical_full_min 0.699