Stable and inert macrocyclic cobalt(II) and nickel(II) complexes with paraCEST response.
Pérez-Lourido, Paulo; Madarasi, Enikő; Antal, Fanni; Esteban-Gómez, David; Wang, Gaoji; Angelovski, Goran; Platas-Iglesias, Carlos; Tircsó, Gyula; Valencia, Laura; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1580–1593; doi:10.1039/d1dt03217h

data_7709139
_publ_section_title
;
 Stable and inert macrocyclic cobalt(II) and nickel(II) complexes with
 paraCEST response.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1580
_journal_page_last               1593
_journal_paper_doi               10.1039/d1dt03217h
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C23 H40 Co N6 O2, 2(F6 P)'
_chemical_formula_sum            'C23 H40 Co F12 N6 O2 P2'
_chemical_formula_weight         781.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-07 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.496(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7343(11)
_cell_length_b                   33.137(3)
_cell_length_c                   17.0102(17)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.47
_cell_volume                     6614.0(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            124186
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.358
_diffrn_reflns_theta_min         2.204
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1020 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.9297. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.223
_platon_squeeze_details
;
TITL shelxt_a.res in P2(1)/n
CELL   11.7343   33.1370   17.0102     90.00     90.50     90.00
SPGR P21/n
C101 0.175 0.986 0.816 !      13.67 eA-3
C102 0.562 0.020 0.850 !       9.88 eA-3
Q103 0.174 0.758 0.624 !       7.02 eA-3
C104 0.828 0.318 0.449 !       5.95 eA-3
Q105 0.075 0.058 0.798 !       2.25 eA-3
Q106 0.168 0.616 0.678 !       2.16 eA-3
Q107 0.581 0.719 0.375 !       1.89 eA-3
Q108 0.816 0.067-0.003 !       1.48 eA-3
Q109 0.262 0.779 0.876 !       1.28 eA-3
Q110 0.939 0.237 0.187 !       1.26 eA-3
Q111 0.533 0.743 0.345 !       1.09 eA-3
Q112 0.395 0.252 0.562 !       1.05 eA-3
Q113 0.050 0.857 0.666 !       1.03 eA-3
Q114 0.843 0.250 0.110 !       0.97 eA-3
Q115 0.781 0.916 0.183 !       0.95 eA-3
Q116 0.096 0.582 0.686 !       0.94 eA-3
Q117 0.312 0.759 0.840 !       0.94 eA-3
Q118 0.981 0.099 0.830 !       0.94 eA-3
Q119 0.300 0.763 0.897 !       0.91 eA-3
Q120 0.079 0.955 0.050 !       0.90 eA-3
Q121 0.812 0.125 0.423 !       0.87 eA-3
Q122 0.173 0.774 0.857 !       0.87 eA-3
Q123 0.827 0.287 0.176 !       0.86 eA-3
Q124 0.829 0.261 0.218 !       0.86 eA-3
Q125 0.171 0.616 0.780 !       0.86 eA-3
Q126 0.172 0.713 0.554 !       0.82 eA-3
Q127 0.675 0.782 0.411 !       0.80 eA-3
Q128 0.327 0.254 0.551 !       0.70 eA-3
Q129 0.092 0.860 0.740 !       0.69 eA-3
Q130 0.920 0.413 0.235 !       0.67 eA-3
Q131 0.033 0.885 0.612 !       0.67 eA-3
Q132 0.673 0.945 0.173 !       0.65 eA-3
Q133 0.241 0.973 0.847 !       0.64 eA-3
Q134 0.861 0.129 0.245 !       0.64 eA-3
Q135 0.816 0.094 0.354 !       0.63 eA-3
Q136 0.379 0.555 0.082 !       0.61 eA-3
Q137 0.308 0.891 0.626 !       0.60 eA-3
Q138 0.610 0.600 0.093 !       0.60 eA-3
Q139 0.261 0.978 0.801 !       0.60 eA-3
Q140 0.783 0.917 0.269 !       0.59 eA-3
Q141 0.987 0.891 0.372 !       0.58 eA-3
Q142 0.674 0.586 0.175 !       0.57 eA-3
Q143 0.207 0.758 0.842 !       0.57 eA-3
Q144 0.187 0.776 0.745 !       0.57 eA-3
Q145 0.155 0.832 0.727 !       0.56 eA-3
Q146 0.861 0.231 0.163 !       0.56 eA-3
Q147 0.156 0.568 0.732 !       0.55 eA-3
Q148 0.813 0.041 0.989 !       0.54 eA-3
Q149 0.766 0.146 0.378 !       0.54 eA-3
Q150 0.189 0.303 0.431 !       0.53 eA-3
Q151 0.229 0.963 0.803 !       0.52 eA-3
Q152 0.296 0.071 0.762 !       0.52 eA-3
Q153 0.457 0.967 0.224 !       0.50 eA-3
;
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         16519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+30.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14316
_reflns_number_total             16519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03217h2.cif
_cod_data_source_block           32019001_0m_sq
_cod_depositor_comments
;
Adding full bibliography for 7709136--7709139.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H80 Co2 F24 N12 O4 P4'
_cod_original_formula_weight         1562.96
_cod_original_formula_moiety         '2(C23 H40 Co N6 O2), 4(F6 P)'
_cod_original_formula_units_Z            4
_cod_database_code               7709139
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3a), N9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,
 H11b), C12(H12a,H12b), C18(H18a,H18b), C29(H29a,H29b), C30(H30a,H30b),
 C31(H31a,H31b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b), C35(H35a,H35b),
  C41(H41a,H41b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C25(H25), C26(H26), C27(H27), N5(H5), N6(H6),
 N11(H11), N12(H12)
2.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C38(H38a,H38b,H38c), C39(H39a,
 H39b,H39c), C40(H40a,H40b,H40c), C44(H44a,H44b,H44c), C45(H45a,H45b,H45c),
 C46(H46a,H46b,H46c)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'