Molecular Quadripod as a Noncovalent Interfacial Coupling Reagent for Forming Immobilized Coordination Assemblies.
Tang, Jian-Hong; Cai, Zhenfeng; Yan, Dong; Tang, Kun; Shao, Jiang-Yang; Zhan, Chuanlang; Wang, Dong; Zhong, Yu-Wu; Wan, Li-Jun; Yao, Jiannian; Journal of the American Chemical Society 140 (2018) 12337–12340; doi:10.1021/jacs.8b07777

data_4132997
_publ_section_title
;
 Molecular Quadripod as a Noncovalent Interfacial Coupling Reagent for
 Forming Immobilized Coordination Assemblies.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12337
_journal_page_last               12340
_journal_paper_doi               10.1021/jacs.8b07777
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C104 H70 N12'
_chemical_formula_sum            'C104 H70 N12'
_chemical_formula_weight         1487.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                93.6740(10)
_cell_angle_beta                 117.5410(10)
_cell_angle_gamma                117.376(3)
_cell_formula_units_Z            1
_cell_length_a                   14.594(4)
_cell_length_b                   15.377(4)
_cell_length_c                   15.584(4)
_cell_measurement_reflns_used    7473
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4707
_cell_measurement_theta_min      1.5930
_cell_volume                     2578.0(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 40.2418
	          2theta: -20.1602
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 40.2418
	          2theta: -20.1602
scan:
	Number of images: 328
	           Slice: -110.0000 - 54.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 40.2418
	          2theta: -20.1602
;
_diffrn_measurement_device
;
?
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0356
_diffrn_orient_matrix_UB_12      -0.0753
_diffrn_orient_matrix_UB_13      0.0408
_diffrn_orient_matrix_UB_21      -0.0371
_diffrn_orient_matrix_UB_22      -0.0407
_diffrn_orient_matrix_UB_23      0.0555
_diffrn_orient_matrix_UB_31      -0.0137
_diffrn_orient_matrix_UB_32      -0.0722
_diffrn_orient_matrix_UB_33      -0.0239
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33648
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         1.574
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_description       plate
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         11751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.1058
_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^)+(0.1499P)^2^+1.2706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2978
_refine_ls_wR_factor_ref         0.3107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9517
_reflns_number_total             11751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07777_si_002.cif
_cod_data_source_block           mx3506c_sq
_cod_original_cell_volume        2577.9(12)
_cod_database_code               4132997
_diffrn_number_total             11756
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C00A(H00A), C10(H10), C21(H21), C46(H46), C9(H9), C45(H45),
 C23(H23), C20(H20), C24(H24), C13(H13), C34(H34), C43(H43), C42(H42), C35(H35),
  C12(H12), C16(H16), C15(H15), C32(H32), C31(H31), C18(H18), C40(H40),
 C39(H39), C29(H29), C17(H17), C37(H37), C48(H48), C38(H38), C28(H28), C51(H51),
  C26(H26), C27(H27), C49(H49), C50(H50)
;
_shelx_res_checksum              74740
_shelx_hkl_checksum              74980
_shelx_fab_checksum              83715
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'