Mechanochemical synthesis of mechanical bonds in M12L8 poly-[<i>n</i>]-catenanes.
Martí-Rujas, Javier; Elli, Stefano; Sacchetti, Alessandro; Castiglione, Franca; Dalton transactions (Cambridge, England : 2003) 51 (2021) 53–58; doi:10.1039/d1dt03158a

data_7709063
_publ_section_title
;
 Mechanochemical synthesis of mechanical bonds in M12L8
 poly-[<i>n</i>]-catenanes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              53
_journal_page_last               58
_journal_paper_doi               10.1039/d1dt03158a
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety
'7.56(C6 H4 Cl2), C168 H120 Br24 N24 Zn12, 6(C2.13 H1.39 Cl0.57), 4.0[C6H4Cl]'
_chemical_formula_sum            'C226.14 H158.58 Br24 Cl18.52 N24 Zn12'
_chemical_formula_weight         6570.91
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-08
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-10-20 deposited with the CCDC.	2021-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   37.9184(11)
_cell_length_b                   37.9184(11)
_cell_length_c                   16.6172(9)
_cell_measurement_reflns_used    7793
_cell_measurement_temperature    98.(2)
_cell_measurement_theta_max      73.7112
_cell_measurement_theta_min      2.3280
_cell_volume                     20691.3(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      98.00
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.477
_diffrn_reflns_theta_min         2.980
_exptl_absorpt_coefficient_mu    7.527
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10108
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.230
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         9386
_refine_ls_number_restraints     1713
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+411.7291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7230
_reflns_number_total             9386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03158a3.cif
_cod_data_source_block           2021s007_tpbznbr2_JMR
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7709063.cif.
;
_cod_original_cell_volume        20691.3(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7709063
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
3. Restrained planarity
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.2 within 2A
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: with sigma of 0.5 and sigma for terminal atoms of 1
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Zn1_1) = Uanis(Zn11_11)
Uanis(Zn2_1) = Uanis(Zn12_11)
5. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Same fragment restrains
7. Others
 Sof(Zn11)=Sof(Br11)=Sof(Br12)=Sof(Zn12)=Sof(Br13)=Sof(Br14)=1-FVAR(1)
 Sof(Zn1)=Sof(Br1)=Sof(Br2)=Sof(Zn2)=Sof(Br3)=Sof(Br4)=FVAR(1)
 Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(N14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=1-FVAR(2)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(N4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(2)
 Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(N14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=1-FVAR(3)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(N4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(3)
 Sof(C6)=Sof(H6)=FVAR(4)
 Sof(C5)=Sof(H5)=FVAR(5)
 Sof(C4)=Sof(H4)=FVAR(6)
 Sof(C3)=Sof(H3)=FVAR(7)
 Fixed Sof: Cl1(0.86) Cl2(0.86) C3(0.86) C4(0.86) C5(0.86) H5(0.86) C6(0.86)
 H6(0.86) C7(0.86) H7(0.86) C8(0.86) H8(0.86) Cl11(0.4) Cl12(0.4) C11(0.4)
 C12(0.4) C13(0.4) H13(0.4) C14(0.4) H14(0.4) C15(0.4) H15(0.4) C16(0.4)
 H16(0.4)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8),
 C10(H10), C12(H12), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
 C6(H6), C8(H8), C2(H2), C3(H3), C5(H5), C6(H6), C3(H3), C4(H4), C5(H5), C6(H6),
  C12(H12), C13(H13), C15(H15), C16(H16), C12(H12), C13(H13), C15(H15),
 C16(H16), C13(H13), C14(H14), C15(H15), C16(H16)
8.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C11(C12,C13,N14,C15,C16), C11(C12,C13,N14,C15,C16),
 C11(C12,C13,C14,C15,C16)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 423 electrons were 
found in a volume of 1302\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 4.0[C6H4Cl] per Formula Unit 
which account for 456 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42979
_shelx_fab_checksum              13811
_olex2_submission_special_instructions 'No special instructions were received'