The crystal packing, morphology and hydrophobicity of polyoxometalate-based amphiphilic materials
Wang, Yu; Lin, Xinjun; Huang, Bo; Chen, Weizhou; Xiao, Zicheng; Wu, Pingfan; CrystEngComm  (2020) –; doi:10.1039/D0CE00129E

data_7240129
_publ_section_title
;
 The crystal packing, morphology and hydrophobicity of
 polyoxometalate-based amphiphilic materials
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00129E
_journal_year                    2020
_chemical_formula_moiety         'C35 H60 N O12.5 V3, C4 H9 N O, C8 H20 N'
_chemical_formula_sum            'C47 H89 N3 O13.5 V3'
_chemical_formula_weight         1065.03
_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
_audit_creation_date             2017-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-12-30 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                99.871(4)
_cell_angle_beta                 90.774(4)
_cell_angle_gamma                117.159(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1207(4)
_cell_length_b                   10.7427(5)
_cell_length_c                   27.9069(12)
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.7390
_cell_volume                     2645.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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     39.00  66.00   1.00   30.00    --    9.97  57.00  90.00   27
  2  \w    -20.00  84.00   1.00   30.00    --    9.97  77.00  60.00  104
  3  \w     49.00  76.00   1.00   30.00    --    9.97 178.00 150.00   27
  4  \w    -38.00  61.00   1.00   30.00    --  -11.85  57.00 -60.00   99
  5  \w    -88.00  10.00   1.00   30.00    --  -11.85 -77.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186840000
_diffrn_orient_matrix_UB_12      -0.0540776000
_diffrn_orient_matrix_UB_13      0.0035982000
_diffrn_orient_matrix_UB_21      0.0607156000
_diffrn_orient_matrix_UB_22      0.0271858000
_diffrn_orient_matrix_UB_23      -0.0142300000
_diffrn_orient_matrix_UB_31      0.0473060000
_diffrn_orient_matrix_UB_32      0.0455187000
_diffrn_orient_matrix_UB_33      0.0213893000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24023
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.658
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             1138
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0289P)^2^+1.8102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8402
_reflns_number_total             11088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00129e2.cif
_cod_data_source_block           35-wo
_cod_original_formula_sum        'C47 H89 N3 O13.50 V3'
_cod_database_code               7240129
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'V O C N'
_reflns_odcompleteness_completeness 96.38
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14A) = Uanis(O14)
Uanis(C44A) = Uanis(C44)
Uanis(C56) = Uanis(C5A)
Uanis(C63) = Uanis(C63A)
Uanis(C5) = Uanis(C56A)
Uanis(N43A) = Uanis(N43)
3. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C44A)=Sof(O14A)=Sof(N43A)=
 Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=1-FVAR(1)
 Sof(O14)=Sof(N43)=Sof(C44)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C65(H65A,H65B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 N15(H15), C24(H24), C27(H27), C31(H31)
4.d Idealised Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C5A(H5AA,H5AB,H5AC)
4.e Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C3(H3A,H3B,
 H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C63A(H63D,H63E,H63F), C56A(H56D,H56E,H56F)
;
_olex2_date_sample_data_collection 2017-12-03
_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 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.591