Expanding medicinal chemistry into 3D space: metallofragments as 3D scaffolds for fragment-based drug discovery
Morrison, Christine N.; Prosser, Kathleen E.; Stokes, Ryjul W.; Cordes, Anna; Metzler-Nolte, Nils; Cohen, Seth M.; Chemical Science 11 (2020) 1216–1225; doi:10.1039/C9SC05586J

data_1556540
_publ_section_title
;
 Expanding medicinal chemistry into 3D space: metallofragments as 3D
 scaffolds for fragment-based drug discovery
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1216
_journal_page_last               1225
_journal_paper_doi               10.1039/C9SC05586J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C13 H11 N2 O6 Re'
_chemical_formula_sum            'C13 H11 N2 O6 Re'
_chemical_formula_weight         477.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2019-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                70.669(2)
_cell_angle_beta                 80.012(2)
_cell_angle_gamma                61.781(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1080(5)
_cell_length_b                   9.5099(5)
_cell_length_c                   9.7673(5)
_cell_measurement_reflns_used    5139
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.288
_cell_measurement_theta_min      2.538
_cell_volume                     703.28(7)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.671
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0785 before and 0.0368 after correction. The Ratio of minimum to maximum transmission is 0.6459. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Light Yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_description       Block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0165P)^2^+0.0535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2647
_reflns_number_total             2866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05586j2.cif
_cod_data_source_block           K9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_colour_modifier' value 'Light' was changed
to 'light' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_colour_primary' value 'Yellow' was changed
to 'yellow' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1556536--1556540.cif.

 Adding full bibliography for 1556536--1556540.cif.
;
_cod_database_code               1556540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.523
_shelx_estimated_absorpt_t_min   0.406
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Re1) = Uanis(Re1B)
Uanis(O4) = Uanis(O5B)
Uanis(O5) = Uanis(O4B)
Uanis(O6) = Uanis(O6B)
Uanis(C6B) = Uanis(C7)
Uanis(C7B) = Uanis(C6)
Uanis(C5) = Uanis(C8B)
Uanis(C8) = Uanis(C5B)
Uanis(C9) = Uanis(C9B)
Uanis(C4) = Uanis(C4B)
Uanis(C2B) = Uanis(C3)
Uanis(O3) = Uanis(O2B)
Uanis(C3B) = Uanis(C2)
Uanis(O3B) = Uanis(O2)
3. Same fragment restrains
{Re1, O2, O3, O4, O5, O6, C2, C3, C4, C5, C6, C7, C8, C9} sigma for 1-2: 0.005,
1-3: 0.005
as
{Re1B, O2B, O3B, O4B, O5B, O6B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B}
4. Others
 Sof(Re1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C2B)=Sof(C3B)=
 Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(C7B)=Sof(C8B)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=1-FVAR(1)
 Sof(Re1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C2)=Sof(C3)=Sof(C4)=
 Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C4(H4), C5(H5), C4B(H4B), C5B(H5B)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C9B(H9BA,H9BB,H9BC)
;
_shelx_res_checksum              58396
_olex2_submission_special_instructions 'No special instructions were received'