Formation of Giant and Small Cyclic Complexes from a Flexible Tripeptide Ligand Controlled by Metal Coordination and Hydrogen Bonds.
Miyake, Ryosuke; Ando, Akira; Ueno, Manami; Muraoka, Takahiro; Journal of the American Chemical Society 141 (2019) 8675–8679; doi:10.1021/jacs.9b01541

data_4127270
_publ_section_title
;
 Formation of Giant and Small Cyclic Complexes from a Flexible Tripeptide
 Ligand Controlled by Metal Coordination and Hydrogen Bonds.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8675
_journal_page_last               8679
_journal_paper_doi               10.1021/jacs.9b01541
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C48 H100 N36 Ni8 O48.5'
_chemical_formula_weight         2427.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.984(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.769(2)
_cell_length_b                   42.392(9)
_cell_length_c                   21.858(5)
_cell_measurement_reflns_used    3310
_cell_measurement_temperature    93
_cell_measurement_theta_max      22.0243
_cell_measurement_theta_min      2.5200
_cell_volume                     9965(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection
'Bruker Instrument Servise 2015.5.1.3/26 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'XSHELL V 6.3.1 (Bruker AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22065
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Tourbo X-ray Source'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.708
_refine_ls_abs_structure_details
;

Flack x determined using 1977 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         13248
_refine_ls_number_restraints     1550
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+102.8285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                9341
_reflns_number_total             13248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01541_si_003.cif
_cod_data_source_block           180822miyake7NiNO3_M8L4_7cm
_cod_depositor_comments          'Adding full bibliography for 4127270.cif.'
_cod_original_cell_volume        9965.(4)
_cod_database_code               4127270
_shelx_res_checksum              78034
_shelx_hkl_checksum              39111