In situ X-ray snapshot analysis of transient molecular adsorption in a crystalline channel
Ryou Kubota; Shohei Tashiro; Motoo Shiro; Mitsuhiko Shionoya; Nature Chemistry 6 (2014) 913–918; doi:10.1038/nchem.2044

data_1551975
_publ_section_title
;
 In situ X-ray snapshot analysis of transient molecular adsorption in a
 crystalline channel
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              913
_journal_page_last               918
_journal_paper_doi               10.1038/nchem.2044
_journal_volume                  6
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C42 H42 Cl6 N6 Pd3, 0.651(C8 H9 Cl O), 1.495(C2 H3 N), 0.629(H2 O)'
_chemical_formula_sum            'C49.81 H53.02 Cl6.65 N7.3 O1.28 Pd3'
_chemical_formula_weight         1329.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.6660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3263(3)
_cell_length_b                   52.7504(10)
_cell_length_c                   19.7460(4)
_cell_measurement_reflns_used    156462
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     14921.4(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            223634
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.014
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5281
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.592
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 15353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.088(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2330
_refine_ls_number_reflns         67147
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                41219
_reflns_number_total             67147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3_x.cif
_cod_data_source_block           X-ray-snapshot-3rd-after-squeeze
_cod_depositor_comments
;

2022-12-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         5318.26
_cod_original_formula_moiety
'4(C42 H42 Cl6 N6 Pd3), 2.606(C8 H9 Cl O), 5.99(C2 H3 N), 2.517(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C199.25 H212.09 Cl26.61 N29.20 O5.12 Pd12'
_cod_database_code               1551975
_shelx_estimated_absorpt_t_min   0.595
_shelx_estimated_absorpt_t_max   0.934