Secondary hierarchical complexity in double-stranded cluster helicates covered by NNNNN type pincer ligands
Xiao, Wang-Chuan; Nie, Qing-Bin; Luo, Geng-Geng; Dalton Transactions  (2023) –; doi:10.1039/D3DT00912B

data_7712847
_publ_section_title
;
 Secondary hierarchical complexity in double-stranded cluster helicates
 covered by NNNNN type pincer ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00912B
_journal_year                    2023
_chemical_formula_moiety         'C70 H46 Ag4 N10'
_chemical_formula_sum            'C70 H46 Ag4 N10'
_chemical_formula_weight         1458.65
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2023-04-18 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4174(2)
_cell_length_b                   17.4174(2)
_cell_length_c                   18.9309(3)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.0490
_cell_measurement_theta_min      3.3640
_cell_volume                     5742.99(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -98.00 -72.00   1.00    0.15    --  -48.20-123.00  26.00   26
  2  \w    -39.00  -9.00   1.00    0.15    --  -48.20 123.00 107.00   30
  3  \w    -90.00 -65.00   1.00    0.15    --  -48.20 150.00 -89.00   25
  4  \w   -116.00 -53.00   1.00    0.15    --  -48.20-150.00-135.00   63
  5  \w     46.00  71.00   1.00    0.15    --   48.20-123.00  26.00   25
  6  \w     45.00  96.00   1.00    0.15    --   48.20-150.00-135.00   51
  7  \w   -140.00-115.00   1.00    0.50    --  -86.25-123.00  26.00   25
  8  \w    -90.00 -65.00   1.00    0.50    --  -86.25 150.00 -89.00   25
  9  \w   -128.00-103.00   1.00    0.50    --  -86.25-150.00-135.00   25
 10  \w    -47.00 -22.00   1.00    0.50    --  -86.25 123.00 107.00   25
 11  \w     37.00 114.00   1.00    0.50    --  106.49-123.00  26.00   77
 12  \w     99.00 125.00   1.00    0.50    --  106.49 123.00 107.00   26
 13  \w     50.00 133.00   1.00    0.50    --  106.49-150.00-135.00   83
 14  \w   -120.00 -25.00   1.00    0.15    --  -48.20 -77.00 120.00   95
 15  \w     37.00 129.00   1.00    0.50    --  106.49 -77.00   0.00   92
 16  \w     94.00 177.00   1.00    0.50    --  106.49  19.00 120.00   83
 17  \w     32.00 119.00   1.00    0.50    --  106.49 -19.00-180.00   87
 18  \w     36.00 120.00   1.00    0.50    --  106.49 -38.00 150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0465428000
_diffrn_orient_matrix_UB_12      0.0340477000
_diffrn_orient_matrix_UB_13      0.0618021000
_diffrn_orient_matrix_UB_21      -0.0271924000
_diffrn_orient_matrix_UB_22      0.0811466000
_diffrn_orient_matrix_UB_23      -0.0205024000
_diffrn_orient_matrix_UB_31      -0.0701200000
_diffrn_orient_matrix_UB_32      -0.0087758000
_diffrn_orient_matrix_UB_33      0.0488387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18744
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.493
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+20.7506P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2694
_reflns_number_total             2969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00912b2.cif
_cod_data_source_block           190520c
_cod_original_cell_volume        5742.99(16)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7712847
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         AgCN
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.238
_diffrn_oxdiff_ac3_digest_frames
;
01c53ed8e98d0d6ddee275383e536e4f9b0094716df
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C20(H20), C4(H4), C5(H5), C21(H21), C14(H14), C6(H6),
 C15(H15), C18(H18), C16(H16), C17(H17)
;
_shelx_res_checksum              19797
_shelx_hkl_checksum              52905
_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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.685