Six-coordinate Iron(II) and Cobalt(II) paraSHIFT Agents for Measuring Temperature by Magnetic Resonance Spectroscopy.
Tsitovich, Pavel B.; Cox, Jordan M.; Benedict, Jason B.; Morrow, Janet R.; Inorganic chemistry 55 (2016) 700–716; doi:10.1021/acs.inorgchem.5b02144

data_4344568
_publ_section_title
;
 Six-coordinate Iron(II) and Cobalt(II) paraSHIFT Agents for Measuring
 Temperature by Magnetic Resonance Spectroscopy.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              700
_journal_page_last               716
_journal_paper_doi               10.1021/acs.inorgchem.5b02144
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C27 H36 Fe N6), C4 F12 Na O12 S4, C F3 O3 S, 0.5(H2 O)'
_chemical_formula_sum            'C59 H73 F15 Fe2 N12 Na O15.5 S5'
_chemical_formula_weight         1778.28
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.079(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0975(17)
_cell_length_b                   13.7505(16)
_cell_length_c                   37.868(4)
_cell_measurement_temperature    90
_cell_volume                     7299.3(14)
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microfocus rotating anode'
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            160296
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1033 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.9285.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3652
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.449(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1987
_refine_ls_number_reflns         40994
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+7.1197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                34715
_reflns_number_total             40994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02144_si_004.cif
_cod_data_source_block           jmc_121404_0m
_cod_depositor_comments
;

2020-10-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         889.14
_cod_original_formula_moiety
'C27 H36 Fe N6, 0.5(C4 F12 Na O12 S4), 0.5(C F3 O3 S), 0.25(H2 O)'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        7299.3(15)
_cod_original_formula_sum
'C29.50 H36.50 F7.50 Fe N6 Na0.50 O7.75 S2.50'
_cod_database_code               4344568
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O31(H31a,H31b)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C17(H17a,H17b),
 C18(H18a,H18b), C19(H19a,H19b), C26(H26a,H26b), C27(H27a,H27b), C55(H55a,H55b),
  C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b), C71(H71a,H71b), C72(H72a,
 H72b), C73(H73a,H73b), C80(H80a,H80b), C81(H81a,H81b), C28(H28a,H28b),
 C35(H35a,H35b), C36(H36a,H36b), C37(H37a,H37b), C44(H44a,H44b), C45(H45a,H45b),
  C46(H46a,H46b), C53(H53a,H53b), C54(H54a,H54b), C82(H82a,H82b), C89(H89a,
 H89b), C90(H90a,H90b), C91(H91a,H91b), C98(H98a,H98b), C99(H99a,H99b),
 C100(H10c,H10d), C107(H10h,H10i), C108(H10j,H10k)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22),
 C23(H23), C57(H57), C58(H58), C59(H59), C66(H66), C67(H67), C68(H68), C75(H75),
  C76(H76), C77(H77), C30(H30), C31(H31), C32(H32), C39(H39), C40(H40),
 C41(H41), C48(H48), C49(H49), C50(H50), C84(H84), C85(H85), C86(H86), C93(H93),
  C94(H94), C95(H95), C102(H102), C103(H103), C104(H104)
2.d Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C16(H16a,H16b,H16c), C25(H25a,H25b,H25c), C61(H61a,H61b,
 H61c), C70(H70a,H70b,H70c), C79(H79a,H79b,H79c), C34(H34a,H34b,H34c), C43(H43a,
 H43b,H43c), C52(H52a,H52b,H52c), C88(H88a,H88b,H88c), C97(H97a,H97b,H97c),
 C106(H10e,H10f,H10g)
;
_olex2_submission_special_instructions 'No special instructions were received'