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_1551100
_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
'O4 P, C50 H44 N14 O10, 3(C4 H12 N), 0.5(C2 H3 N)'
_chemical_formula_sum            'C62.25 H80.37 N17.12 O13 P'
_chemical_formula_weight         1307.52
_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
_audit_creation_date             2018-10-13
_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                 94.6020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5380(8)
_cell_length_b                   15.2994(7)
_cell_length_c                   51.669(2)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.86
_cell_measurement_theta_min      2.22
_cell_volume                     16971.0(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture photon II '
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            287127
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         25.068
_diffrn_reflns_theta_min         1.548
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1753 before and 0.0805 after correction.
The Ratio of minimum to maximum transmission is 0.8387.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       BIOCK
_exptl_crystal_F_000             5542
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6250
_platon_squeeze_details
;
;
_refine_diff_density_max         0.786
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1703
_refine_ls_number_reflns         30060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0916
_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^)+(0.1831P)^2^+6.4424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2709
_refine_ls_wR_factor_ref         0.2966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20147
_reflns_number_total             30060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02012h2.cif
_cod_data_source_block           TMA
_cod_depositor_comments
;
The following automatic conversions were performed:

tag '_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 

2022-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         2615.05
_cod_original_formula_moiety
'2(O4 P), 2(C50 H44 N14 O10), 4(C4 H12 N), C4 N, C8 N, C2 H3 N'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        16970.9(12)
_cod_original_formula_sum        'C124.50 H160.75 N34.25 O26 P2'
_cod_database_code               1551100
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.934
_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.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C29(H29A,H29B), C72(H72A,H72B), C79(H79A,H79B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), N3(H3A), N4(H4), N5(H5A), N6(H6A), N7(H7), N8(H8), N9(H9A),
 N10(H10A), N11(H11A), N12(H12A), N13(H13), 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), N16(H16A), N17(H17A), N18(H18A), N19(H19A), N20(H20), N21(H21),
 N22(H22), N23(H23), N24(H24A), N25(H25A), N26(H26), N27(H27A), C52(H52),
 C53(H53), C55(H55), C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C66(H66),
  C67(H67), C68(H68), C69(H69), C74(H74), C75(H75), C77(H77), C78(H78),
 C82(H82), C83(H83), C84(H84), C85(H85), C89(H89), C90(H90), C91(H91), C92(H92),
  C96(H96), C97(H97), C99(H99), C100(H100)
2.c Idealised Me refined as rotating group:
 C101(H10B,H10C,H10D), C102(H10E,H10F,H10G), C103(H10H,H10I,H10J), C104(H10K,
 H10L,H10M), C105(H10N,H10O,H10P), C106(H10Q,H10R,H10S), C107(H10T,H10U,H10V),
 C108(H10W,H10X,H10Y), C109(H,H10Z,HA), C110(H11B,H11C,H11D), C111(H11E,H11F,
 H11G), C112(H11H,H11I,H11J), C117(H11K,H11L,H11M), C118(H11N,H11O,H11P),
 C119(H11Q,H11R,H11S), C120(H12B,H12C,H12D), C125(H12E,H12F,H12G)
;
_olex2_submission_special_instructions 'No special instructions were received'