Allosteric cooperativity in ternary complexes with low symmetry.
Chai, Hongxin; Yang, Liu-Pan; Ke, Hua; Pang, Xin-Yu; Jiang, Wei; Chemical communications (Cambridge, England) 54 (2018) 7677–7680; doi:10.1039/c8cc04195d

data_7121850
_publ_section_title
;
 Allosteric cooperativity in ternary complexes with low symmetry.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7677
_journal_page_last               7680
_journal_paper_doi               10.1039/c8cc04195d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C66 H64 O12, C H2 Cl2'
_chemical_formula_sum            'C67 H66 Cl2 O12'
_chemical_formula_weight         1134.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.884(2)
_cell_angle_beta                 73.714(2)
_cell_angle_gamma                80.961(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3158(4)
_cell_length_b                   12.7690(4)
_cell_length_c                   19.5858(6)
_cell_measurement_reflns_used    7245
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      59.67
_cell_measurement_theta_min      3.51
_cell_volume                     2918.52(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22961
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        58.928
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0747 before and 0.0575 after correction. The Ratio of minimum to maximum transmission is 0.8279. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         8339
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1300P)^2^+0.9129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4922
_reflns_number_total             8339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04195d2.cif
_cod_data_source_block           p-1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7121849--7121850.cif.'
_cod_database_code               7121850
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-C66A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C66B) = Uanis(C66A)
4. Others
 Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(H66C)=1-FVAR(1)
 Sof(H65A)=Sof(H65B)=Sof(C66B)=Sof(H66D)=Sof(H66E)=Sof(H66F)=FVAR(1)
 Fixed Sof: H18A(0.5) H18B(0.5) H19A(0.5) H19B(0.5) H34A(0.5) H34B(0.5)
 H35A(0.5) H35B(0.5) O5A(0.5) O5B(0.5) O7A(0.5) O7B(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C50(H50), C52(H52)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B),
 C19(H19A,H19B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B),
  C35(H35A,H35B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C51(H51A,
 H51B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C65(H65C,H65D),
 C67(H67A,H67B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C12(H12), C13(H13), C21(H21), C22(H22), C26(H26), C27(H27),
 C38(H38), C39(H39), C43(H43), C44(H44), C54(H54), C55(H55), C59(H59), C60(H60)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C49(H49A,H49B,H49C), C66A(H66A,H66B,
 H66C), C66B(H66D,H66E,H66F)
;
_olex2_submission_special_instructions 'No special instructions were received'