Preparation, X-ray Structures, Spectroscopic, and Redox Properties of Di- and Trinuclear Iron-Zirconium and Iron-Hafnium Porphyrinoclathrochelates.
Dudkin, Semyon V.; Erickson, Nathan R.; Vologzhanina, Anna V.; Novikov, Valentin V.; Rhoda, Hannah M.; Holstrom, Cole D.; Zatsikha, Yuriy V.; Yusubov, Mekhman S.; Voloshin, Yan Z.; Nemykin, Victor N.; Inorganic chemistry 55 (2016) 11867–11882; doi:10.1021/acs.inorgchem.6b01936

data_4349132
_publ_section_title
;
 Preparation, X-ray Structures, Spectroscopic, and Redox Properties of Di-
 and Trinuclear Iron-Zirconium and Iron-Hafnium Porphyrinoclathrochelates.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11867
_journal_page_last               11882
_journal_paper_doi               10.1021/acs.inorgchem.6b01936
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C66 H61 B Fe N10 O6 Zr, 0.5(C6 H14)'
_chemical_formula_sum            'C69 H68 B Fe N10 O6 Zr'
_chemical_formula_weight         1291.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.136(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5372(4)
_cell_length_b                   23.9405(5)
_cell_length_c                   17.2239(12)
_cell_measurement_reflns_used    5874
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      61.59
_cell_measurement_theta_min      3.07
_cell_volume                     6212.7(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42454
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       prism
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         14180
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+27.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8192
_reflns_number_total             14180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01936_si_002.cif
_cod_data_source_block           3a
_cod_database_code               4349132
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Others
 Fixed Sof: C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5)
 C4S(0.5) H4SA(0.5) H4SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 Fixed Uiso: H3A(0.034) H3B(0.034) H4A(0.041) H4B(0.041) H5A(0.041) H5B(0.041)
 H6A(0.037) H6B(0.037) H9A(0.036) H9B(0.036) H10A(0.05) H10B(0.05) H11A(0.046)
 H11B(0.046) H12A(0.035) H12B(0.035) H15A(0.032) H15B(0.032) H16A(0.038)
 H16B(0.038) H17A(0.039) H17B(0.039) H18A(0.034) H18B(0.034) H19A(0.035)
 H19B(0.035) H20A(0.044) H20B(0.044) H21A(0.05) H21B(0.05) H22A(0.076)
 H22B(0.076) H22C(0.076) H24(0.04) H25(0.041) H29(0.037) H30(0.039) H34(0.037)
 H35(0.039) H39(0.035) H40(0.038) H48(0.071) H47(0.071) H46(0.071) H45(0.071)
 H44(0.071) H50(0.046) H51(0.058) H52(0.052) H53(0.049) H54(0.039) H60(0.048)
 H59(0.056) H58(0.051) H57(0.054) H56(0.045) H62(0.065) H63(0.065) H64(0.065)
 H65(0.065) H66(0.065) H6SA(0.113) H6SB(0.113) H6SC(0.113) H2SA(0.09)
 H2SB(0.09) H5SA(0.09) H5SB(0.09) H1SA(0.113) H1SB(0.113) H1SC(0.113)
 H4SA(0.09) H4SB(0.09) H3SA(0.09) H3SB(0.09)
 Fixed X: H3A(0.1881) H3B(0.1108) H4A(0.2008) H4B(0.2893) H5A(0.2566)
 H5B(0.1633) H6A(0.2559) H6B(0.3356) H9A(0.2749) H9B(0.3345) H10A(0.4262)
 H10B(0.3962) H11A(0.5394) H11B(0.4969) H12A(0.5083) H12B(0.4726) H15A(-0.0648)
 H15B(-0.0454) H16A(0.0058) H16B(-0.0862) H17A(-0.0053) H17B(0.0159)
 H18A(0.1533) H18B(0.1456) H19A(0.3861) H19B(0.4672) H20A(0.3942) H20B(0.4863)
 H21A(0.5137) H21B(0.4524) H22A(0.5555) H22B(0.6135) H22C(0.6077) H24(-0.0965)
 H25(0.051) H29(0.2828) H30(0.2731) H34(0.068) H35(-0.0436) H39(-0.2336) H40(-
 0.2596) H48(-0.1304) H47(-0.2436) H46(-0.3899) H45(-0.4228) H44(-0.3096)
 H50(0.3038) H51(0.4048) H52(0.3672) H53(0.2287) H54(0.1277) H60(0.1091)
 H59(0.1776) H58(0.2902) H57(0.3344) H56(0.266) H62(-0.0168) H63(-0.0728) H64(-
 0.2257) H65(-0.3226) H66(-0.2666) H6SA(0.481) H6SB(0.5777) H6SC(0.495)
 H2SA(0.4224) H2SB(0.4967) H5SA(0.4881) H5SB(0.5923) H1SA(0.4945) H1SB(0.5522)
 H1SC(0.5858) H4SA(0.609) H4SB(0.5567) H3SA(0.4237) H3SB(0.4723)
 Fixed Y: H3A(0.3978) H3B(0.376) H4A(0.299) H4B(0.3344) H5A(0.2749)
 H5B(0.3059) H6A(0.3459) H6B(0.352) H9A(0.6826) H9B(0.6413) H10A(0.7145)
 H10B(0.7086) H11A(0.6691) H11B(0.6257) H12A(0.5758) H12B(0.6269) H15A(0.5537)
 H15B(0.6081) H16A(0.6574) H16B(0.6296) H17A(0.5556) H17B(0.6151) H18A(0.6196)
 H18B(0.5555) H19A(0.462) H19B(0.4698) H20A(0.5569) H20B(0.5261) H21A(0.6135)
 H21B(0.5992) H22A(0.5356) H22B(0.5408) H22C(0.5922) H24(0.3775) H25(0.3812)
 H29(0.541) H30(0.644) H34(0.7821) H35(0.77) H39(0.5965) H40(0.5024)
 H48(0.3597) H47(0.2928) H46(0.3189) H45(0.4118) H44(0.4787) H50(0.4458)
 H51(0.3887) H52(0.3513) H53(0.3709) H54(0.4279) H60(0.7233) H59(0.7972)
 H58(0.8484) H57(0.8257) H56(0.7518) H62(0.7141) H63(0.7719) H64(0.7876)
 H65(0.7456) H66(0.6879) H6SA(0.7323) H6SB(0.7597) H6SC(0.7966) H2SA(0.5814)
 H2SB(0.5832) H5SA(0.7551) H5SB(0.7635) H1SA(0.5303) H1SB(0.519) H1SC(0.5632)
 H4SA(0.6707) H4SB(0.6714) H3SA(0.6629) H3SB(0.6666)
 Fixed Z: H3A(0.7326) H3B(0.772) H4A(0.7696) H4B(0.8046) H5A(0.9042)
 H5B(0.8952) H6A(1.0067) H6B(0.9631) H9A(0.7997) H9B(0.7613) H10A(0.8191)
 H10B(0.9014) H11A(0.9118) H11B(0.8423) H12A(0.9583) H12B(1.0018) H15A(0.9653)
 H15B(0.9181) H16A(1.0359) H16B(1.0417) H17A(1.1207) H17B(1.1637) H18A(1.1393)
 H18B(1.163) H19A(1.1997) H19B(1.1589) H20A(1.2369) H20B(1.2739) H21A(1.2256)
 H21B(1.1391) H22A(1.1153) H22B(1.2056) H22C(1.1452) H24(0.5734) H25(0.544)
 H29(0.5454) H30(0.5568) H34(0.6729) H35(0.7528) H39(0.8133) H40(0.7523)
 H48(0.7006) H47(0.6785) H46(0.6183) H45(0.5803) H44(0.6024) H50(0.6619)
 H51(0.618) H52(0.4886) H53(0.4031) H54(0.447) H60(0.481) H59(0.4304)
 H58(0.5159) H57(0.652) H56(0.7026) H62(0.897) H63(0.9827) H64(0.9584)
 H65(0.8483) H66(0.7627) H6SA(0.5574) H6SB(0.5732) H6SC(0.5828) H2SA(0.608)
 H2SB(0.6881) H5SA(0.6944) H5SB(0.7033) H1SA(0.5528) H1SB(0.6419) H1SC(0.586)
 H4SA(0.6706) H4SB(0.7402) H3SA(0.6475) H3SB(0.576)
;
_shelx_res_checksum              63199
_shelx_hkl_checksum              79935
_olex2_submission_special_instructions 'No special instructions were received'