Construction and interconversion of anion-coordination-based (‘aniono’) grids and double helicates modulated by counter-cations
Fan, Xiaoxia; Zhang, Dan; Jiang, Shiyu; Wang, Heng; Lin, Lin-Ting; Zheng, Bo; Xu, Wen-Hua; Zhao, Yanxia; Hay, Benjamin P.; Chan, Yi-Tsu; Yang, Xiao-Juan; Li, Xiaopeng; Wu, Biao; Chemical Science  (2019) –; doi:10.1039/C9SC02012H

data_1551102
_publ_section_title
;
 Construction and interconversion of anion-coordination-based
 (&#x2018;aniono&#x2019;) grids and double helicates modulated by
 counter-cations
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02012H
_journal_year                    2019
_chemical_formula_moiety
'C50 H44 N14 O10, 2(C8 H20 N), C3.5 N0.5, O4 P, C4 N0.5, 3(C3 O)'
_chemical_formula_sum            'C85 H126 N17 O17 P'
_chemical_formula_weight         1688.99
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-22 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   35.9168(11)
_cell_length_b                   35.9168(11)
_cell_length_c                   32.8056(14)
_cell_measurement_reflns_used    7891
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      22.5740
_cell_measurement_theta_min      2.1520
_cell_volume                     42320(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      9.00  34.00   0.50   20.00    --    7.20  57.00  60.00   50
  2  \w    -53.00  23.00   0.50   20.00    --   -7.40 -57.00  60.00  152
  3  \w    -97.00 -68.00   0.50   20.00    --   -7.40 -57.00  60.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0149444000
_diffrn_orient_matrix_UB_12      0.0129318000
_diffrn_orient_matrix_UB_13      -0.0001926000
_diffrn_orient_matrix_UB_21      0.0023880000
_diffrn_orient_matrix_UB_22      -0.0024910000
_diffrn_orient_matrix_UB_23      0.0212892000
_diffrn_orient_matrix_UB_31      0.0126985000
_diffrn_orient_matrix_UB_32      -0.0147064000
_diffrn_orient_matrix_UB_33      -0.0037694000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            68954
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             14496
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         18551
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.1007
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.5351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2820
_refine_ls_wR_factor_ref         0.3029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9746
_reflns_number_total             18551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02012h2.cif
_cod_data_source_block           TEA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1551102
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 N17-C69
 1.49 with sigma of 0.02
 C67-N17
 1.49 with sigma of 0.02
 C69-C70
 1.54 with sigma of 0.02
 C67-C68
 1.54 with sigma of 0.02
 C73-C74
 1.54 with sigma of 0.02
 C82-C83
 1.54 with sigma of 0.02
 C82-O17
 1.35 with sigma of 0.02
 C79-O16
 1.35 with sigma of 0.02
 N18-C73
 1.49 with sigma of 0.02
 N18-C71
 1.49 with sigma of 0.02
 N18-C72
 2.2 with sigma of 0.02
 C71-C72
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C69, C70
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N18, C73, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
N18 \\sim C73: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C29(H29A,H29B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,
 H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B),
 C65(H65A,H65B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C27(H27), C28(H28),
  C32(H32), C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41),
 C42(H42), C46(H46), C47(H47), C49(H49), C50(H50), N2(H2A), N3(H3A), N4(H4),
 N5(H5A), N6(H6A), N7(H7), N8(H8), N9(H9A), N10(H10A), N11(H11A), N12(H12A),
 N13(H13)
5.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,
 H66B,H66C)
;
_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 3.532
_oxdiff_exptl_absorpt_empirical_full_min 0.443
_platon_squeeze_void_probe_radius 1.20