Manipulating clusters by regulating N,O chelating ligands: structures and multistep assembly mechanisms
Wang, Hai-Ling; Liu, Zi-Yuan; Zhu, Zhong-Hong; Peng, Jin-Mei; Ma, Xiong-Feng; Bai, Juan; Zou, Hua-Hong; Mo, Kai-Qiang; Liang, Fu-Pei; CrystEngComm 22 (2020) 915–923; doi:10.1039/C9CE01730E

data_7239718
_publ_section_title
;
 Manipulating clusters by regulating N,O chelating ligands: structures and
 multistep assembly mechanisms
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              915
_journal_page_last               923
_journal_paper_doi               10.1039/C9CE01730E
_journal_volume                  22
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H80 Gd9 N16 O50'
_chemical_formula_sum            'C32 H80 Gd9 N16 O50'
_chemical_formula_weight         2904.37
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-12-23 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3000(2)
_cell_length_b                   17.3000(2)
_cell_length_c                   14.4460(3)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8195
_cell_measurement_theta_min      2.9807
_cell_volume                     4323.54(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -24.00   53.00   1.0000    6.2500
omega____ theta____ kappa____ phi______ frames
    -      -16.8791   38.0000    0.0000 77

  2 omega  -91.00  -66.00   1.0000    6.2500
omega____ theta____ kappa____ phi______ frames
    -      -16.8791 -178.0000    0.0000 25

  3 omega  -88.00   20.00   1.0000    6.2500
omega____ theta____ kappa____ phi______ frames
    -      -16.8791  -19.0000   30.0000 108
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0176606000
_diffrn_orient_matrix_UB_12      0.0247981000
_diffrn_orient_matrix_UB_13      -0.0328816000
_diffrn_orient_matrix_UB_21      0.0247462000
_diffrn_orient_matrix_UB_22      -0.0146904000
_diffrn_orient_matrix_UB_23      -0.0349752000
_diffrn_orient_matrix_UB_31      -0.0275032000
_diffrn_orient_matrix_UB_32      -0.0291586000
_diffrn_orient_matrix_UB_33      -0.0103339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16176
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.895
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1644 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.064(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3891
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0333P)^2^+2.8623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.931
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                3728
_reflns_number_total             3891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01730e2.cif
_cod_data_source_block           0925-lfp-xsz-gd
_cod_depositor_comments
;Adding full bibliography for 7239717--7239719.cif.

 Adding full bibliography for 7239717--7239719.cif.
;
_cod_original_cell_volume        4323.57(14)
_cod_database_code               7239718
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.339
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C5-C6 = C7-C8
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 3.8A
with sigma of 0.02 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B), C3(H3C,H3D), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
;
_shelx_res_checksum              84033
_olex2_submission_special_instructions 'No special instructions were received'