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_7239719
_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         'C48 H32 Gd12 N16 O64'
_chemical_formula_sum            'C48 H32 Gd12 N16 O64'
_chemical_formula_weight         3743.89
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_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                   18.4916(16)
_cell_length_b                   18.4916(16)
_cell_length_c                   21.4412(19)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.9274
_cell_measurement_theta_min      2.3847
_cell_volume                     7331.6(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16491
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         1.454
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.417
_exptl_absorpt_correction_T_max  0.06
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.168
_refine_diff_density_min         -4.627
_refine_diff_density_rms         0.309
_refine_ls_abs_structure_details
;
 Flack x determined using 1451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         4200
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0506
_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^)+(0.1071P)^2^+7.9026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3681
_reflns_number_total             4200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01730e2.cif
_cod_data_source_block           aa
_cod_depositor_comments
;Adding full bibliography for 7239717--7239719.cif.

 Adding full bibliography for 7239717--7239719.cif.
;
_cod_original_cell_volume        7331.6(14)
_cod_database_code               7239719
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.058
_shelx_estimated_absorpt_t_min   0.046
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C2
 1.32 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim C1 \\sim C5 \\sim C4 \\sim C2 \\sim C3: within 3.8A with sigma of 0.02
and sigma for terminal atoms of 0.01
O7 \\sim O1 \\sim O2 \\sim O8 \\sim O6 \\sim O5 \\sim O3 \\sim O4: within 3.8A
with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              29292
_olex2_submission_special_instructions 'No special instructions were received'