Precursor control over the self-assembly of [2]catenanes via hydrazone condensation in water.
Wang, Cai-Yun; Wu, Guangcheng; Jiao, Tianyu; Shen, Libo; Ma, Ge; Pan, Yuanjiang; Li, Hao; Chemical communications (Cambridge, England) 54 (2018) 5106–5109; doi:10.1039/c8cc02599a

data_7121548
_publ_section_title
;
 Precursor control over the self-assembly of [2]catenanes via hydrazone
 condensation in water.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5106
_journal_page_last               5109
_journal_paper_doi               10.1039/c8cc02599a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '10(F6 P), 4(C39 H38 N6 O2), F5 P, C2 H3 N'
_chemical_formula_sum            'C158 H155 F65 N25 O8 P11'
_chemical_formula_weight         4107.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                100.067(10)
_cell_angle_beta                 91.197(10)
_cell_angle_gamma                90.025(10)
_cell_formula_units_Z            2
_cell_length_a                   18.275(3)
_cell_length_b                   22.178(4)
_cell_length_c                   26.090(4)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      51.01
_cell_measurement_theta_min      3.70
_cell_volume                     10409(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      170.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            156365
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.182
_diffrn_reflns_theta_min         2.957
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1579 before and 0.1041 after correction.
The Ratio of minimum to maximum transmission is 0.6754.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.774
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2406
_refine_ls_number_reflns         39674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.774
_refine_ls_R_factor_all          0.2410
_refine_ls_R_factor_gt           0.1828
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4861
_refine_ls_wR_factor_ref         0.5211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19903
_reflns_number_total             39674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02599a2.cif
_cod_data_source_block           mjl18033_0m
_cod_depositor_comments
'Adding full bibliography for 7121548--7121549.cif.'
_cod_database_code               7121548
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.797
_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:
 C03M(H03A,H03B), C03W(H03D,H03G), C044(H04A,H04B), C045(H04Q,H04T), C04A(H04X,
 H04), C04T(H04C,H04D), C04U(H04E,H04F), C04W(H04I,H04K), C04X(H04O,H04P),
 C052(H05N,H05O), C054(H05Z,H), C056(H05,HA), C059(H5AA,HB), C05B(H05F,H05G),
 C05C(H05H,H05I), C05F(H05J,H05K), C05G(H05Q,H05R), C05K(H7AA,HC), C05O(H05V,
 H05W), C05P(H05A,H05B), C05Q(H05X,H05Y), C05R(H05C,H05E), C05S(H8AA,HD),
 C05X(H9AA,HE), C05Y(H05L,H05M), C060(H06A,H06B), C061(H06C,H06D), C06A(H06E,
 H06F)
2.b Aromatic/amide H refined with riding coordinates:
 N00U(H00U), N00W(H00W), N014(H014), N015(H015), N019(H019), N01B(H01B),
 C01C(H01C), C01J(H01J), C01K(H01K), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01W(H01W), C01X(H01X), N01Z(H01Z), C020(H020), C021(H021),
 C024(H024), C027(H027), C029(H029), C02B(H02B), C02D(H02D), C02E(H02E),
 C02G(H02G), C02I(H02I), C02M(H02M), C02O(H02O), C02P(H02P), C02Q(H02Q),
 N02R(H02R), C02S(H02S), C02U(H02U), C02V(H02V), C02W(H02W), C02Y(H02Y),
 C031(H031), C032(H032), C035(H035), C037(H037), C038(H038), C03A(H03C),
 C03B(H03H), C03C(H03L), C03E(H03E), C03F(H03F), C03G(H03M), C03H(H03T),
 C03I(H03I), C03J(H03J), C03K(H03K), C03L(H03W), C03N(H03N), C03O(H03O),
 C03P(H03P), C03Q(H03Q), C03R(H03R), C03S(H03S), C03U(H03U), C03V(H03V),
 C03Y(H03Y), C03Z(H03Z), C041(H041), C042(H042), C043(H043), C046(H046),
 C047(H047), C048(H048), C049(H049), C04C(H0AA), C04D(H04L), C04E(H04M),
 C04F(H04U), C04G(H04G), C04H(H04H), C04I(H1AA), C04J(H04J), C04L(H04N),
 C04M(H2AA), C04N(H3AA), C04O(H4AA), C04P(H04W), C04R(H04R), C04S(H04S),
 C04V(H04V), C04Y(H04Y), C04Z(H04Z), C053(H053), C055(H055), C058(H058),
 C05A(H6AA), C05D(H05D), C05E(H05P), C05H(H05S), C05I(H05T), C05J(H05U)
2.c Idealised Me refined as rotating group:
 C062(H06G,H06H,H06I)
;
_shelx_res_checksum              68738
_shelx_fab_checksum              42908
_olex2_submission_special_instructions 'No special instructions were received'