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_7045404
_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
'C92 H108 Cl4 N8 O16 Pd2, 2(C36 H32 N4), 2(Cl4 Zn), 10(H2 O), 8(Cl)'
_chemical_formula_sum            'C164 H192 Cl20 N16 O26 Pd2 Zn2'
_chemical_formula_weight         3855.86
_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             2015-08-05
_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                91.369(2)
_cell_angle_beta                 90.147(2)
_cell_angle_gamma                97.5953(19)
_cell_formula_units_Z            1
_cell_length_a                   12.2761(4)
_cell_length_b                   19.5771(7)
_cell_length_c                   20.4123(8)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.331
_cell_measurement_theta_min      2.301
_cell_volume                     4861.2(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58662
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.519
_diffrn_reflns_theta_min         0.998
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1037 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.8398.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       needle
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         20008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1151P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12458
_reflns_number_total             20008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04792d2.cif
_cod_data_source_block           cx0532
_cod_depositor_comments
'Adding full bibliography for 7045404--7045405.cif.'
_cod_database_code               7045404
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.992
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1S(H1SA,H1SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB), O4S(H4SA,H4SB), O5S(H5SA,H5SB)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C11(H11A,H11B), C18(H18A,H18B), C29(H29A,
 H29B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
 C46(H46), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C73(H73),
  C74(H74), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C82(H82), C1(H1),
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35)
;
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 836.3 Ang^3^ [17.0%]
Total electron count / cell = 302.5

The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.
;
_shelx_res_checksum              20824
_olex2_date_sample_data_collection 2015-08-04
_olex2_date_sample_submission    2015-07-27
_olex2_submission_original_sample_id cx0532
_olex2_submission_special_instructions 'No special instructions were received'