Anisotropic coordination star polymers realized by self-sorting core modulation
Hosono, Nobuhiko; Omoto, Kenichiro; Kitagawa, Susumu; Chem. Commun.  (2017) –; doi:10.1039/C7CC04381C

data_7120392
_publ_section_title
;
 Anisotropic coordination star polymers realized by self-sorting core
 modulation
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04381C
_journal_year                    2017
_chemical_formula_moiety         'C156 H120 Cu12 N12 O60'
_chemical_formula_sum            'C156 H120 Cu12 N12 O60'
_chemical_formula_weight         3885.11
_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             2017-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-05 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                107.9914(18)
_cell_angle_beta                 99.9315(16)
_cell_angle_gamma                108.1284(18)
_cell_formula_units_Z            1
_cell_length_a                   20.1292(4)
_cell_length_b                   21.7528(4)
_cell_length_c                   22.5286(4)
_cell_measurement_reflns_used    22959
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.5590
_cell_measurement_theta_min      1.8690
_cell_volume                     8513.8(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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79367
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.664
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku XtaLAB P200'
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.758
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method N,N-Diethylformamide
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.641
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00017(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         42004
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1647P)^2^+3.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25911
_reflns_number_total             42004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04381c2.cif
_cod_data_source_block           AzoMOP-tBuipa6
_cod_database_code               7120392
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C11, C10, C9, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C35, C34, C33, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C10 \\sim C12 \\sim C9: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.08
C35 \\sim C34 \\sim C33 \\sim C36: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.08
4.a Aromatic/amide H refined with riding coordinates:
 C55(H55), C69(H69), C4(H4), C77(H77), C14(H14), C16(H16), C18(H18), C63(H63),
 C73(H73), C51(H51), C75(H75), C41(H41), C6(H6), C65(H65), C2(H2), C49(H49),
 C53(H53), C52(H52), C74(H74), C28(H28), C47(H47), C67(H67), C59(H59), C61(H61),
  C66(H66), C45(H45), C26(H26), C39(H39), C30(H30), C46(H46), C37(H37),
 C60(H60), C38(H38)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C11(H11A,
 H11B,H11C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              26133
_shelx_hkl_checksum              91873
_shelx_fab_checksum              99515
_olex2_submission_special_instructions 'No special instructions were received'