Selective Binding and Quantitation of Calcium with a Cobalt-Based Magnetic Resonance Probe.
Du, Kang; Thorarinsdottir, Agnes E.; Harris, T. David; Journal of the American Chemical Society 141 (2019) 7163–7172; doi:10.1021/jacs.9b02661

data_4128114
_publ_section_title
;
 Selective Binding and Quantitation of Calcium with a Cobalt-Based
 Magnetic Resonance Probe.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7163
_journal_page_last               7172
_journal_paper_doi               10.1021/jacs.9b02661
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'2(C26 H34 Co N4 O8), C3 H6 O, 2(H1.18 O0.55)'
_chemical_formula_sum            'C55 H76.36 Co2 N8 O18.1'
_chemical_formula_weight         1257.12
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   35.066(7)
_cell_length_b                   35.066(7)
_cell_length_c                   35.066(7)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      2.17
_cell_volume                     43118(15)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            293059
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         1.161
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             15869
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.167
_refine_diff_density_max         2.276
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7358
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0805
_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^)+(0.1427P)^2^+356.2265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5013
_reflns_number_total             7358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02661_si_002.cif
_cod_data_source_block           LCo_apo
_cod_original_cell_volume        43118(27)
_cod_original_formula_sum        'C55 H76.36 Co2 N8 O18.10'
_cod_database_code               4128114
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.870
_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, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C3AA-C2AA
 1.54 with sigma of 0.005
 O2AA-C25 = O2AA-C2AA = O18-C5AA
 1.43 with sigma of 0.005
 O0AA-C0AA = O0AA-C1AA = O1AA-C6 = O1AA-C25
 1.43 with sigma of 0.005
 C6-C1AA = C7-C0AA
 1.53 with sigma of 0.005
 O3AA-C3AA
 1.43 with sigma of 0.005
 O3AA-C4AA
 1.43 with sigma of 0.01
 C5AA-C4AA
 1.53 with sigma of 0.005
3. Rigid bond restraints
 C5AA, C3AA, C2AA, O2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C0AA, O0AA, C1AA, C6, O1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5AA, C4AA, O3AA, C3AA, C2AA, O2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4AA, O3AA, C3AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5AA, C4AA, O3AA, C3AA, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4AA \\sim C0AA \\sim O0AA \\sim O3AA \\sim C3AA \\sim C1AA: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4AA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C7) = Uanis(C5AA)
Uanis(C0AA) = Uanis(C4AA)
Uanis(O0AA) = Uanis(O3AA)
Uanis(C1AA) = Uanis(C3AA)
Uanis(C6) = Uanis(C2AA)
Uanis(O1AA) = Uanis(O2AA)
5. Others
 Sof(H25C)=Sof(H25D)=Sof(O2AA)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(C3AA)=
 Sof(H3AA)=Sof(H3AB)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(C4AA)=Sof(H4AA)=
 Sof(H4AB)=Sof(O3AA)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(O1AA)=Sof(O0AA)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=
 FVAR(1)
 Fixed Sof: H4AC(0.59) H4AD(0.59)
6.a Free rotating group:
 O4AA(H4AC,H4AD)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C15(H15A,H15B), C17(H17A,H17B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C25(H25C,H25D), C29(H29A,H29B), C34(H34A,H34B), C6(H6A,
 H6B), C7(H7A,H7B), C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C5AA(H5AA,H5AB),
 C3AA(H3AA,H3AB), C2AA(H2AA,H2AB), C4AA(H4AA,H4AB)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C27(H27), C28(H28), C31(H31), C32(H32), C35(H35)
6.d X=CH2 refined with riding coordinates:
 N12(H12A,H12B), N30(H30A,H30B)
6.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              23735
_shelx_hkl_checksum              50032
_shelx_fab_checksum              14744
_olex2_submission_special_instructions 'No special instructions were received'