Studies towards the synthesis of Pd(ii)-containing [2] and [3]catenanes in aqueous media.
López-Vidal, E M; Prokofjevs, A.; Gibbs-Hall, I C; Dale, E. J.; Quintela, J. M.; Peinador, C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2492–2496; doi:10.1039/c7dt04792d

data_7045405
_publ_section_title
;
 Studies towards the synthesis of Pd(ii)-containing [2] and [3]catenanes
 in aqueous media.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2492
_journal_page_last               2496
_journal_paper_doi               10.1039/c7dt04792d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C46 H54 Cl6 N4 O8 Zn2, C36 H32 N4, 2(Cl4 Zn), 3(O), 3(H2 O)'
_chemical_formula_sum            'C82 H92 Cl14 N8 O14 Zn4'
_chemical_formula_weight         2171.41
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-12-19 deposited with the CCDC.
2018-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                105.917(3)
_cell_angle_beta                 91.108(3)
_cell_angle_gamma                105.758(3)
_cell_formula_units_Z            2
_cell_length_a                   14.5280(10)
_cell_length_b                   16.6911(12)
_cell_length_c                   20.7097(14)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.653
_cell_measurement_theta_min      3.620
_cell_volume                     4623.9(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55819
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.694
_diffrn_reflns_theta_min         2.230
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.432
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.6146.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.595
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16113
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1102P)^2^+17.7325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14227
_reflns_number_total             16113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04792d2.cif
_cod_data_source_block           cx0479
_cod_depositor_comments
'Adding full bibliography for 7045404--7045405.cif.'
_cod_database_code               7045405
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.228
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3S-H3SB = O3S-H3SA
 0.87 with sigma of 0.001
 H3SB-H3SA
 1.42 with sigma of 0.001
3.a Free rotating group:
 O5S(H5SA,H5SB), O6S(H6SA,H6SB)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C1A(H1AA,H1AB), C8A(H8AA,H8AB), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C36(H36A,H36B), C29A(H29C,H29D), C30A(H30C,H30D), C31A(H31C,
 H31D), C32A(H32C,H32D), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A),
  C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A),
 C17A(H17A), C18A(H18A), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C38(H38), C39(H39), C40(H40), C19A(H19A),
 C20A(H20A), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C27A(H27A),
 C28A(H28A), C38A(H38A), C39A(H39A), C40A(H40A)
;
_shelx_res_checksum              10137
_olex2_date_sample_data_collection 2015-06-18
_olex2_date_sample_submission    2015-06-16
_olex2_submission_original_sample_id cx0479
_olex2_submission_special_instructions 'No special instructions were received'