Self-assembly of cuprous iodide cluster-based calix[4]resorcinarenes and photocatalytic properties
Hu, Chu-Xing; Xuan, Ya-Hui; Jiang, Zi-Hao; Lu, Tao; Yang, Jie; Yuan, Hui; Tian, You-Ping; Sun, Zheng-Guang; Jiang, Xuan-Feng; CrystEngComm 23 (2021) 7179–7185; doi:10.1039/D1CE01069G

data_7243637
_publ_section_title
;
 Self-assembly of cuprous iodide cluster-based calix[4]resorcinarenes and
 photocatalytic properties
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              7179
_journal_page_last               7185
_journal_paper_doi               10.1039/D1CE01069G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C124 H110 Cu8 I8 N10 O16 S8 [+ solvent]'
_chemical_formula_sum            'C124 H110 Cu8 I8 N10 O16 S8'
_chemical_formula_weight         3776.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2021-02-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.557(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.5046(17)
_cell_length_b                   16.0447(6)
_cell_length_c                   23.0476(14)
_cell_measurement_reflns_used    7375
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.9310
_cell_measurement_theta_min      2.1270
_cell_volume                     7174.2(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.8518
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  27.00   1.00    8.50    --  -11.59 -99.00  90.00   27
  2  \w      9.00  86.00   1.00    8.50    --   11.74  37.00 -30.00   77
  3  \w    -64.00  42.00   1.00    8.50    --   11.74 -77.00-150.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0355794000
_diffrn_orient_matrix_UB_12      -0.0072089000
_diffrn_orient_matrix_UB_13      -0.0094171000
_diffrn_orient_matrix_UB_21      -0.0060255000
_diffrn_orient_matrix_UB_22      0.0008314000
_diffrn_orient_matrix_UB_23      -0.0327717000
_diffrn_orient_matrix_UB_31      0.0058113000
_diffrn_orient_matrix_UB_32      -0.0436264000
_diffrn_orient_matrix_UB_33      0.0009559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.1618
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.8518
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40013
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.8518
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             6125.884
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.5602
_refine_diff_density_min         -2.6117
_refine_diff_density_rms         0.3869
_refine_ls_d_res_high            0.7181
_refine_ls_d_res_low             9.7003
_refine_ls_goodness_of_fit_ref   0.9434
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    92
_refine_ls_number_parameters     789
_refine_ls_number_reflns         17265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9434
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -29
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -15
_reflns_number_gt                9481
_reflns_number_total             17265
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce01069g2.cif
_cod_data_source_block           hcx-cu
_cod_depositor_comments
'Adding full bibliography for 7243636--7243637.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7243637
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C27(H27), C38(H38), C52(H52)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C15(H15a,H15b), C19(H19a,H19b), C30(H30a,H30b), C36(H36a,H36b),
 C37(H37a,H37b), C46(H46a,H46b), C54(H54a,H54b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C11(H11), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22), C23(H23),
 C24(H24), C35(H35), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C56(H56),
  C57(H57), C59(H59), C60(H60), C126(H126)
2.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C29(H29a,H29b,H29c), C39(H39a,H39b,H39c), C53(H53a,H53b,
 H53c), C61(H61a,H61b,H61c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.391
_oxdiff_exptl_absorpt_empirical_full_min 0.453