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_4128113
_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         'C27 H38 Ca Co N5 O12, 2(C H4 O), N O3'
_chemical_formula_sum            'C29 H46 Ca Co N6 O17'
_chemical_formula_weight         849.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7639(7)
_cell_length_b                   21.7165(14)
_cell_length_c                   31.819(2)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      2.85
_cell_volume                     7437.8(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.11
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            234999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.265
_diffrn_reflns_theta_min         1.280
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.8603
_exptl_absorpt_correction_T_min  0.8227
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         11030
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.1350
_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^)+(0.0001P)^2^+115.3634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2840
_refine_ls_wR_factor_ref         0.2880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9688
_reflns_number_total             11030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02661_si_004.cif
_cod_data_source_block           LCoCa(NO3)2
_cod_original_cell_volume        7437.9(8)
_cod_database_code               4128113
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O13A-C28A
 1.43 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O12-H12A
 0.87 with sigma of 0.01
 C27B-H12
 1.944241 with sigma of 0.02
 Ca1-H12
 2.972448 with sigma of 0.02
 C27A-H12A
 2.004179 with sigma of 0.02
 Ca1-H12A
 2.809853 with sigma of 0.02
 O13B-C28B \\sim O13A-C28A
 with sigma of 0.01
3. Rigid bond restraints
 O13A, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O13B, C28B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O13A \\sim O13B \\sim C28A \\sim C28B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Others
 Sof(O15B)=1-FVAR(1)
 Sof(O15A)=FVAR(1)
 Sof(O13B)=Sof(H13B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(O13A)=Sof(H13A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
 Sof(N4B)=1-FVAR(3)
 Sof(N4A)=FVAR(3)
 Sof(O14A)=1-FVAR(4)
 Sof(O14B)=FVAR(4)
 Sof(H12A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(5)
 Sof(H12)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12B,H12C),
 C14(H14A,H14B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C16(H16), C17(H17), C18(H18)
6.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4A(H4AA,H4AB)
6.d Idealised Me refined as rotating group:
 C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F), C28A(H28A,H28B,H28C), C28B(H28D,
 H28E,H28F), C29(H29A,H29B,H29C)
6.e Idealised tetrahedral OH refined as rotating group:
 O13A(H13A), O13B(H13B), O17(H17A)
;
_shelx_res_checksum              91040
_shelx_hkl_checksum              17637
_olex2_submission_special_instructions 'No special instructions were received'