Imidazole-Appended Macrocyclic Complexes of Fe(II), Co(II), and Ni(II) as ParaCEST Agents.
Burns, Patrick J.; Cox, Jordan M.; Morrow, Janet R.; Inorganic chemistry 56 (2017) 4546–4555; doi:10.1021/acs.inorgchem.7b00176

data_4345786
_publ_section_title
;
 Imidazole-Appended Macrocyclic Complexes of Fe(II), Co(II), and Ni(II) as
 ParaCEST Agents.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4546
_journal_page_last               4555
_journal_paper_doi               10.1021/acs.inorgchem.7b00176
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C18 H30 N6 Ni O3, 2(C F3 O3 S)'
_chemical_formula_sum            'C20 H30 F6 N6 Ni O9 S2'
_chemical_formula_weight         735.33
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-01 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 110.9092(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3644(9)
_cell_length_b                   13.3889(6)
_cell_length_c                   22.2130(9)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.157
_cell_measurement_theta_min      2.275
_cell_volume                     5657.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Bruker APEX2 area detector'
_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       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51602
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0652 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.8807.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         11588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0305P)^2^+9.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8713
_reflns_number_total             11588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00176_si_004.cif
_cod_data_source_block           jmc_041602_0m
_cod_database_code               4345786
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4(0.017) H6(0.019) H1A(0.018) H1B(0.018) H2A(0.018) H2B(0.018)
 H3A(0.018) H3B(0.018) H4A(0.019) H4B(0.019) H5A(0.02) H5B(0.02) H6A(0.018)
 H6B(0.018) H7A(0.018) H7B(0.018) H8A(0.022) H8B(0.022) H9A(0.018) H9B(0.018)
 H10A(0.017) H10B(0.017) H11A(0.015) H11B(0.015) H13(0.017) H14(0.015)
 H15A(0.018) H15B(0.018) H17(0.021) H18(0.018) H10(0.024) H12(0.029)
 H19A(0.029) H19B(0.029) H20A(0.034) H20B(0.034) H21A(0.037) H21B(0.037)
 H22A(0.039) H22B(0.039) H23A(0.034) H23B(0.034) H24A(0.032) H24B(0.032)
 H25A(0.031) H25B(0.031) H26A(0.03) H26B(0.03) H27A(0.03) H27B(0.03)
 H28A(0.027) H28B(0.027) H29A(0.022) H29B(0.022) H31(0.023) H32(0.021)
 H33A(0.027) H33B(0.027) H35(0.033) H36(0.028)
 Fixed X: H4(0.333) H6(0.4394) H1A(0.2077) H1B(0.1823) H2A(0.2432) H2B(0.1827)
 H3A(0.2684) H3B(0.3148) H4A(0.3894) H4B(0.3602) H5A(0.479) H5B(0.5087)
 H6A(0.5399) H6B(0.5759) H7A(0.5729) H7B(0.5271) H8A(0.4944) H8B(0.4864)
 H9A(0.3639) H9B(0.3576) H10A(0.2483) H10B(0.2764) H11A(0.3132) H11B(0.2517)
 H13(0.4314) H14(0.4733) H15A(0.5103) H15B(0.5307) H17(0.3109) H18(0.2638)
 H10(0.869) H12(0.4894) H19A(0.5761) H19B(0.6249) H20A(0.6655) H20B(0.5811)
 H21A(0.5919) H21B(0.6746) H22A(0.6217) H22B(0.5678) H23A(0.6085) H23B(0.6661)
 H24A(0.7577) H24B(0.7063) H25A(0.7691) H25B(0.8024) H26A(0.8017) H26B(0.7305)
 H27A(0.709) H27B(0.77) H28A(0.6782) H28B(0.6214) H29A(0.7768) H29B(0.7409)
 H31(0.9083) H32(0.819) H33A(0.6248) H33B(0.6423) H35(0.4158) H36(0.4974)
 Fixed Y: H4(0.8044) H6(1.102) H1A(0.9472) H1B(0.8824) H2A(0.9952) H2B(1.0512)
 H3A(1.2092) H3B(1.13) H4A(1.2528) H4B(1.224) H5A(1.1757) H5B(1.1983)
 H6A(1.0296) H6B(1.0697) H7A(0.8725) H7B(0.8649) H8A(0.7273) H8B(0.7931)
 H9A(0.7281) H9B(0.6854) H10A(0.75) H10B(0.8402) H11A(0.7399) H11B(0.8026)
 H13(0.9088) H14(0.9999) H15A(0.9405) H15B(1.0537) H17(1.1263) H18(1.0525)
 H10(0.8949) H12(0.4656) H19A(0.7851) H19B(0.8645) H20A(0.9273) H20B(0.9322)
 H21A(0.9247) H21B(0.8998) H22A(0.8237) H22B(0.7654) H23A(0.6043) H23B(0.6436)
 H24A(0.5827) H24B(0.4928) H25A(0.4224) H25B(0.5313) H26A(0.4783) H26B(0.4154)
 H27A(0.5254) H27B(0.6047) H28A(0.6966) H28B(0.6446) H29A(0.7693) H29B(0.8728)
 H31(0.8506) H32(0.731) H33A(0.4327) H33B(0.4221) H35(0.6016) H36(0.7145)
 Fixed Z: H4(0.5419) H6(0.9605) H1A(0.7173) H1B(0.6524) H2A(0.6069)
 H2B(0.6247) H3A(0.6418) H3B(0.6197) H4A(0.6881) H4B(0.7442) H5A(0.8117)
 H5B(0.755) H6A(0.7527) H6B(0.8251) H7A(0.8435) H7B(0.7681) H8A(0.8138)
 H8B(0.8714) H9A(0.8335) H9B(0.7639) H10A(0.7412) H10B(0.7912) H11A(0.6669)
 H11B(0.615) H13(0.5382) H14(0.6422) H15A(0.9086) H15B(0.8991) H17(0.9234)
 H18(0.8147) H10(0.6126) H12(0.6076) H19A(0.4741) H19B(0.4559) H20A(0.5621)
 H20B(0.5334) H21A(0.648) H21B(0.6747) H22A(0.7422) H22B(0.6812) H23A(0.7185)
 H23B(0.7849) H24A(0.7525) H24B(0.7537) H25A(0.6775) H25B(0.6799) H26A(0.5835)
 H26B(0.5688) H27A(0.4632) H27B(0.4983) H28A(0.4252) H28B(0.4497) H29A(0.5034)
 H29B(0.511) H31(0.7281) H32(0.736) H33A(0.6684) H33B(0.6038) H35(0.544)
 H36(0.5176)
;
_olex2_submission_special_instructions 'No special instructions were received'