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_7712846
_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         'C35 H25 N5, H2 O'
_chemical_formula_sum            'C35 H27 N5 O'
_chemical_formula_weight         533.61
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-18
_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                 110.215(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8674(14)
_cell_length_b                   13.0593(9)
_cell_length_c                   15.2619(12)
_cell_measurement_reflns_used    2341
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      24.0240
_cell_measurement_theta_min      3.9050
_cell_volume                     2780.7(4)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.845
_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    -33.00  42.00   1.00   22.50    --  -16.28  55.00 -10.00   75
  2  \w    -20.00  48.00   1.00   22.50    --  -16.28  77.00  60.00   68
  3  \w     35.00  88.00   1.00   22.50    --   15.49 178.00 -30.00   53
  4  \w    -23.00  21.00   1.00   22.50    --  -16.28 -99.00 120.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218086000
_diffrn_orient_matrix_UB_12      0.0471741000
_diffrn_orient_matrix_UB_13      -0.0042671000
_diffrn_orient_matrix_UB_21      -0.0182797000
_diffrn_orient_matrix_UB_22      0.0226745000
_diffrn_orient_matrix_UB_23      0.0326096000
_diffrn_orient_matrix_UB_31      0.0421536000
_diffrn_orient_matrix_UB_32      -0.0145453000
_diffrn_orient_matrix_UB_33      0.0369968000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14155
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.408
_diffrn_reflns_theta_min         3.429
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.120
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.0047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0396P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2759
_reflns_number_total             6480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00912b2.cif
_cod_data_source_block           exp_6881
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712846
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.984
_reflns_odcompleteness_completeness 99.61
_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 N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O(HA,HB)
2.b Aromatic/amide H refined with riding coordinates:
 N1AA(H1AA), N2AA(H2AA), C1BA(H1BA), C2BA(H2BA), C4BA(H4BA), C7BA(H7BA),
 C8BA(H8BA), C9BA(H9BA), C0CA(H0CA), C3CA(H3CA), C5CA(H5CA), C6CA(H6CA),
 C7CA(H7CA), C9CA(H9CA), C0DA(H0DA), C1DA(H1DA), C2DA(H2DA), C3DA(H3DA),
 C4DA(H4DA), C5DA(H5DA), C6DA(H6DA), C7DA(H7DA), C8DA(H8DA), C9DA(H9DA),
 C0EA(H0EA)
;
_shelx_res_checksum              86955
_shelx_hkl_checksum              31895
_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 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.590