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_1544630
_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         'C40 H48 B4 Fe2 N14 O12, 3(C H2 Cl2)'
_chemical_formula_sum            'C43 H54 B4 Cl6 Fe2 N14 O12'
_chemical_formula_weight         1326.64
_chemical_name_systematic
;
 ?
;
_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   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                60.961(8)
_cell_angle_beta                 79.048(8)
_cell_angle_gamma                87.787(7)
_cell_formula_units_Z            2
_cell_length_a                   8.4174(8)
_cell_length_b                   19.6607(14)
_cell_length_c                   20.1792(15)
_cell_measurement_reflns_used    3954
_cell_measurement_temperature    140.0(2)
_cell_measurement_theta_max      75.2830
_cell_measurement_theta_min      4.3810
_cell_volume                     2860.9(5)
_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_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_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            20081
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.084
_diffrn_reflns_theta_min         4.426
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.241
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         11426
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+8.1421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8126
_reflns_number_total             11426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           L2
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_database_code               1544630
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl6A-C3S = Cl6B-C3S
 1.75 with sigma of 0.02
 Cl6B-C3S
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5) \\sim Ueq, Uanis(C3S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
4. Others
 Fixed Sof: H3SA(0.5) H3SB(0.5) H3SC(0.5) H3SD(0.5) Cl6A(0.5) Cl6B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C3S(H3SC,H3SD), C2S(H2SA,H2SB), C1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
 C4AA(H4AA), C13(H13), C15(H15), C16(H16), C17(H17), C19(H19), C21(H21),
 C22(H22), C35(H35), C37(H37), C38(H38), C39(H39)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              54782
_shelx_hkl_checksum              37893
_olex2_submission_special_instructions 'No special instructions were received'