Poly(ethylene glycol) modified Mn2+ complexes as contrast agents with a prolonged observation window in rat MRA
Wu, Changqiang; Yang, Li; Chen, Zhuzhong; Zhang, Houbing; Li, Danyang; Lin, Bingbing; Zhu, Jiang; Ai, Hua; Zhang, Xiaoming; RSC Advances 7 (2017) 54603–; doi:10.1039/C7RA09975D

data_7229626
_publ_section_title
;
 Poly(ethylene glycol) modified Mn2+ complexes as contrast agents with a
 prolonged observation window in rat MRA
;
_journal_issue                   86
_journal_name_full               'RSC Advances'
_journal_page_first              54603
_journal_paper_doi               10.1039/C7RA09975D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C51 H69 Mn4 N9 O15, 2(Cl), 3(H2 O)'
_chemical_formula_sum            'C51 H75 Cl2 Mn4 N9 O18'
_chemical_formula_weight         1392.86
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-18 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0674(8)
_cell_length_b                   13.2889(6)
_cell_length_c                   35.945(2)
_cell_measurement_reflns_used    3119
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      26.3385
_cell_measurement_theta_min      2.7637
_cell_volume                     6241.9(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      145.15
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -90.00  -64.00   0.4000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7361  162.0000   37.0000 65

  2 omega   24.00   79.20   0.4000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611   38.0000 -180.0000 138

  3 omega    2.00   66.00   0.4000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611   38.0000  -90.0000 160
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0227344000
_diffrn_orient_matrix_UB_12      -0.0022433000
_diffrn_orient_matrix_UB_13      -0.0179099000
_diffrn_orient_matrix_UB_21      -0.0478910000
_diffrn_orient_matrix_UB_22      0.0134280000
_diffrn_orient_matrix_UB_23      0.0078217000
_diffrn_orient_matrix_UB_31      0.0114809000
_diffrn_orient_matrix_UB_32      0.0516138000
_diffrn_orient_matrix_UB_33      -0.0028160000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.1282
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            14832
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         3.169
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_F_000             2888
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ????'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1784 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.665
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    0.878
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                6400
_reflns_number_total             9866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09975d1.cif
_cod_data_source_block           1
_cod_database_code               7229626
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C30H40N4O2Mn1
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.764
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H31A,H31B} of C31, {H29A,H29B} of C29, {H37A,H37B} of C37,
   {H23A,H23B} of C23, {H20A,H20B} of C20, {H40A,H40B} of C40, {H30A,H30B} of
  C30, {H22A,H22B} of C22, {H32A,H32B} of C32, {H38A,H38B} of C38, {H39A,H39B}
  of C39, {H21A,H21B} of C21, {H48A,H48B} of C48, {H47A,H47B} of C47, {H46A,
  H46B} of C46, {H49A,H49B} of C49, {H3A,H3B} of C3, {H4C,H4D} of C4, {H6A,H6B}
  of C6, {H5A,H5B} of C5, {H14A,H14B} of C14, {H15C,H15D} of C15, {H12A,H12B}
  of C12, {H13A,H13B} of C13
 At 1.5 times of:
  All O(H,H) groups, {H17A,H17B} of C51
2. Restrained distances
 O4-H4B = O4-H4A
 0.85 with sigma of 0.02
 O11-H11B = O11-H11A
 0.85 with sigma of 0.02
 O15-H15A = O15-H15B
 0.85 with sigma of 0.02
 O17-H17A = O17-H17B
 0.85 with sigma of 0.02
 H4A-H4B
 1.39 with sigma of 0.04
 H11A-H11B
 1.39 with sigma of 0.04
 H15B-H15A
 1.39 with sigma of 0.04
 H17B-H17A
 1.39 with sigma of 0.04
 Mn1-H4B \\sim Mn1-H4A
 with sigma of 0.02
 Mn4-H11B \\sim Mn4-H11A
 with sigma of 0.02
 Mn3-H15A \\sim Mn3-H15B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) =
Uanis(N8) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28)
Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C47) = Uanis(C48) = Uanis(C49)
4.a Free rotating group:
 O16(H16A,H16B), O18(H18A,H18B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C16(H16), C19(H19), C33(H33), C36(H36), C50(H50)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B), C6(H6A,H6B), C12(H12A,H12B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15C,H15D), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B)
4.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C25(H25), C26(H26), C27(H27), C42(H42), C43(H43),
 C44(H44)
;
_olex2_submission_special_instructions 'No special instructions were received'