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_1556536
_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_absolute_configuration ad
_chemical_formula_moiety         'C15 H13 N2 O5 Re'
_chemical_formula_sum            'C15 H13 N2 O5 Re'
_chemical_formula_weight         487.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3450(2)
_cell_length_b                   14.5492(5)
_cell_length_c                   16.7909(7)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.820
_cell_measurement_theta_min      2.426
_cell_volume                     1550.05(10)
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17683
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         1.852
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.866
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0956 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.5858. 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    2.089
_exptl_crystal_description       Rod
_exptl_crystal_F_000             928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM, hexanes'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0072P)^2^+1.4757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2054
_reflns_number_total             3161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05586j2.cif
_cod_data_source_block           K5
_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               1556536
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.285
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Shared sites
{C8B, N2}
{C8, N2B}
3. Uiso/Uaniso restraints and constraints
Uanis(C8B) = Uanis(N2)
Uanis(C8) = Uanis(N2B)
4. Others
 Sof(N2B)=Sof(H4B)=Sof(H7B)=Sof(H9BD)=Sof(H9BE)=Sof(H9BF)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C8B)=1-FVAR(1)
 Sof(N2)=Sof(H4A)=Sof(H7A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C8)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C4(H4B), C7(H7A), C7(H7B), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15)
5.b Idealised Me refined as rotating group:
 C9(H9AA,H9AB,H9AC), C9(H9BD,H9BE,H9BF), C10(H10A,H10B,H10C), C10(H10D,H10E,
 H10F)
;
_shelx_res_checksum              16665
_olex2_submission_special_instructions 'No special instructions were received'