PdII2L4-type coordination cages up to three nanometers in size
Jansze, Suzanne M.; Wise, Matthew D.; Vologzhanina, Anna V.; Scopelliti, Rosario; Severin, Kay; Chem. Sci. 8 (2017) 1901–; doi:10.1039/C6SC04732G

data_1544629
_publ_section_title
;
 PdII2L4-type coordination cages up to three nanometers in size
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              1901
_journal_paper_doi               10.1039/C6SC04732G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C52 H60 B4 Fe2 N14 O12, 4(C H2 Cl2)'
_chemical_formula_sum            'C56 H68 B4 Cl8 Fe2 N14 O12'
_chemical_formula_weight         1567.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-10-21 deposited with the CCDC.
2016-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.174(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4453(5)
_cell_length_b                   15.7177(2)
_cell_length_c                   23.5873(7)
_cell_measurement_reflns_used    11799
_cell_measurement_temperature    140.0(2)
_cell_measurement_theta_max      75.3460
_cell_measurement_theta_min      3.6820
_cell_volume                     6809.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50099
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.192
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.887
_exptl_absorpt_correction_T_max  0.622
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'light red'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.744
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.097
_refine_diff_density_max         2.124
_refine_diff_density_min         -2.649
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         14020
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0848
_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^)+(0.0200P)^2^+48.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10452
_reflns_number_total             14020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           L1
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_database_code               1544629
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl9-C4S \\sim Cl8-C4S \\sim Cl7-C4S
 with sigma of 0.02
 Cl7-Cl8 \\sim Cl7-Cl9 \\sim Cl8-Cl9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C45) = Uiso(C45A)
Uiso(C46) = Uiso(C46A)
Uanis(Cl9) = Uanis(Cl8) = Uanis(Cl7)
4. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1AC(0.5) H1AD(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) H44D(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 C45A(0.5) H45C(0.5) H45D(0.5) C46A(0.5) H46C(0.5) H46D(0.5) Cl7(0.66667)
 Cl8(0.66667) Cl9(0.66667) H4SC(0.5) H4SD(0.5) H4SA(0.5) H4SB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C1AA(H1AC,H1AD), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C44(H44A,H44B), C44(H44C,H44D),
 C45(H45A,H45B), C46(H46A,H46B), C45A(H45C,H45D), C46A(H46C,H46D), C2S(H2SA,
 H2SB), C3S(H3SA,H3SB), C1S(H1SA,H1SB), C4S(H4SC,H4SD), C4S(H4SA,H4SB)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27), C28(H28),
 C29(H29), C47(H47), C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              47872
_shelx_hkl_checksum              61476
_olex2_submission_special_instructions 'No special instructions were received'