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_7121549
_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
'16(F3 P0.5), 4(C42 H36 N6 O2), 12(C2 H3 N), 2(O)'
_chemical_formula_sum            'C192 H180 F48 N36 O10 P8'
_chemical_formula_weight         4311.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 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                90
_cell_angle_beta                 105.457(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3375(10)
_cell_length_b                   27.6556(8)
_cell_length_c                   43.5292(12)
_cell_measurement_reflns_used    9384
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.72
_cell_measurement_theta_min      3.748
_cell_volume                     39841(2)
_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      169.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            216258
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.003
_diffrn_reflns_theta_min         2.788
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1030 before and 0.0701 after correction. The Ratio of minimum to maximum transmission is 0.7621. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             17728
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2661
_refine_ls_number_reflns         37789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+128.0663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26739
_reflns_number_total             37789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02599a2.cif
_cod_data_source_block           mjl18032_0m
_cod_depositor_comments
'Adding full bibliography for 7121548--7121549.cif.'
_cod_database_code               7121549
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.902
_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:
 C028(H02A,H02B), C029(H02D,H02E), C048(H04A,H04D), C04F(H04G,H04H), C057(H05A,
 H05B), C05J(H05I,H05J), C064(H06Q,H06S), C068(H06U,H06V), C06E(H06E,H06F),
 C06P(H06N,H06P), C06Y(H06A,H06B), C06Z(H06C,H06D), C071(H07A,H07B), C073(H07C,
 H07D), C074(H07E,H07F), C078(H07G,H07H)
2.b Aromatic/amide H refined with riding coordinates:
 N00T(H00T), N00W(H00W), N011(H011), N016(H016), N01D(H01D), N01I(H01I),
 N01L(H01L), N01V(H01V), C022(H022), C027(H027), C02B(H02C), C02D(H02F),
 C02E(H02G), C02F(H02H), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L),
 C02M(H02M), C02N(H02N), C02P(H02P), C02R(H02R), C02T(H02T), C02V(H02V),
 C02Y(H02Y), C030(H030), C031(H031), C032(H032), C034(H034), C038(H038),
 C039(H039), C03A(H03A), C03B(H03B), C03E(H03E), C03J(H03J), C03L(H03L),
 C03O(H03O), C03P(H03P), C03S(H03S), C03W(H03W), C03Y(H03Y), C040(H040),
 C041(H041), C042(H042), C043(H043), C044(H044), C045(H045), C046(H046),
 C049(H049), C04A(H04E), C04B(H04B), C04C(H04C), C04D(H04F), C04G(H04L),
 C04H(H04M), C04I(H04I), C04J(H04J), C04K(H04K), C04M(H04N), C04O(H04O),
 C04P(H04P), C04Q(H04Q), C04S(H04S), C04U(H04U), C04X(H04X), C04Y(H04Y),
 C04Z(H04Z), C050(H050), C051(H051), C052(H052), C053(H053), C056(H056),
 C058(H058), C05A(H05C), C05C(H05D), C05D(H05E), C05E(H05F), C05F(H05K),
 C05G(H05G), C05H(H05H), C05K(H05M), C05L(H05L), C05M(H05P), C05N(H05N),
 C05O(H05O), C05P(H05R), C05Q(H05Q), C05S(H05S), C05U(H05U), C05V(H05V),
 C05W(H05W), C05X(H05X), C05Y(H05Y), C062(H062), C065(H065), C067(H067),
 C069(H069), C06A(H06G), C06B(H06I), C06C(H06W), C06D(H06J), C06F(H06L),
 C06H(H06H), C06I(H06X), C06J(H06M), C06K(H06K), C06L(H06Y), C06M(H06Z),
 C06O(H06O), C06R(H06R), C06T(H06T), C06U(H06)
2.c Idealised Me refined as rotating group:
 C07E(H07R,H07S,H07T), C07N(H07O,H07P,H07Q), C07V(H07L,H07M,H07N), C07X(H07I,
 H07J,H07K), C07Y(H07U,H07V,H07W), C080(H08G,H08H,H08I), C081(H08J,H08K,H08L),
 C082(H08M,H08N,H08O), C083(H08D,H08E,H08F), C086(H08A,H08B,H08C), C087(H08S,
 H08T,H08U), C088(H08P,H08Q,H08R)
;
_shelx_res_checksum              26274
_olex2_submission_special_instructions 'No special instructions were received'