Conformational control of Pd2L4 assemblies with unsymmetrical ligands
Lewis, James E. M.; Tarzia, Andrew; White, Andrew J. P.; Jelfs, Kim E.; Chemical Science 11 (2020) 677–683; doi:10.1039/C9SC05534G

data_1557105
_publ_section_title
;
 Conformational control of Pd2L4 assemblies with unsymmetrical ligands
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              677
_journal_page_last               683
_journal_paper_doi               10.1039/C9SC05534G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C88 H56 N8 Pd2, 4(B F4), 4(C4 H10 O)'
_chemical_formula_sum            'C104 H96 B4 F16 N8 O4 Pd2'
_chemical_formula_weight         2081.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6541(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3600(4)
_cell_length_b                   12.35285(17)
_cell_length_c                   27.6660(4)
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.7860
_cell_measurement_theta_min      4.2760
_cell_volume                     9660.2(2)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15734
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.463
_diffrn_reflns_theta_min         3.905
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.749
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+8.4784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7879
_reflns_number_total             9259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05534g2.cif
_cod_data_source_block           cis-Pd2_2_4-BF4_4
_cod_depositor_comments
'Adding full bibliography for 1557105--1557106.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1557105
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              35411
_shelx_fab_checksum              17254