Sterically induced reductive linkage of iron polypnictides with bulky lanthanide complexes by ring-opening of THF.
Schoo, Christoph; Bestgen, Sebastian; Schmidt, Monika; Konchenko, Sergey N.; Scheer, Manfred; Roesky, Peter W.; Chemical communications (Cambridge, England) 52 (2016) 13217–13220; doi:10.1039/c6cc07367k

data_7125186
_publ_section_title
;
 Sterically induced reductive linkage of iron polypnictides with bulky
 lanthanide complexes by ring-opening of THF.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13217
_journal_page_last               13220
_journal_paper_doi               10.1039/c6cc07367k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C118 H171 Fe N8 O2 P5 Sm2, C7 H16'
_chemical_formula_sum            'C125 H187 Fe N8 O2 P5 Sm2'
_chemical_formula_weight         2345.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.08.15 svn.r3327 for OlexSys, GUI svn.r5212)
;
_audit_update_record
;
2016-09-08 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                109.26(3)
_cell_angle_beta                 93.54(3)
_cell_angle_gamma                93.97(3)
_cell_formula_units_Z            2
_cell_length_a                   13.120(3)
_cell_length_b                   20.386(4)
_cell_length_c                   24.637(5)
_cell_measurement_reflns_used    46381
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.59
_cell_volume                     6181(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
'STOE X-RED & X-SHAPE, PLATON (A.L.Spek, 2009)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56801
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.135
_diffrn_reflns_theta_min         1.591
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.9067
_exptl_absorpt_correction_T_min  0.7005
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1326
_refine_ls_number_reflns         23995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17066
_reflns_number_total             23995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07367k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6180(2)
_cod_database_code               7125186
_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
2.a Ternary CH refined with riding coordinates:
 C40(H40), C15(H15), C12(H12), C52(H52), C84(H84), C109(H109), C37(H37),
 C72(H72), C100(H100), C27(H27), C75(H75), C49(H49), C24(H24), C97(H97),
 C87(H87), C112(H112)
2.b Secondary CH2 refined with riding coordinates:
 C118(H11D,H11E), C4(H4A,H4B), C3(H3A,H3B), C117(H11F,H11G), C2(H2A,H2B),
 C1(H1A,H1B), C115(H11K,H11L), C116(H11S,H11T), C120(H12A,H12B), C121(H12C,
 H12D), C123(H12E,H12F), C122(H12G,H12H), C124(H12L,H12M)
2.c Me refined with riding coordinates:
 C125(H12I,H12J,H12K)
2.d Aromatic/amide H refined with riding coordinates:
 C46(H46), C5(H5), C106(H106), C65(H65), C30(H30), C45(H45), C20(H20),
 C47(H47), C93(H93), C9(H9), C68(H68), C35(H35), C90(H90), C80(H80), C95(H95),
 C22(H22), C34(H34), C81(H81), C70(H70), C107(H107), C10(H10), C69(H69),
 C21(H21), C33(H33), C8(H8), C105(H105), C82(H82), C94(H94)
2.e Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C54(H54A,H54B,
 H54C), C113(H11A,H11B,H11C), C50(H50A,H50B,H50C), C28(H28A,H28B,H28C),
 C25(H25A,H25B,H25C), C61(H61A,H61B,H61C), C13(H13A,H13B,H13C), C42(H42A,H42B,
 H42C), C14(H14A,H14B,H14C), C76(H76A,H76B,H76C), C88(H88A,H88B,H88C), C73(H73A,
 H73B,H73C), C98(H98A,H98B,H98C), C38(H38A,H38B,H38C), C60(H60A,H60B,H60C),
 C62(H62A,H62B,H62C), C86(H86A,H86B,H86C), C51(H51A,H51B,H51C), C17(H17A,H17B,
 H17C), C99(H99A,H99B,H99C), C101(H10A,H10B,H10C), C114(H11H,H11I,H11J),
 C77(H77A,H77B,H77C), C102(H10D,H10E,H10F), C89(H89A,H89B,H89C), C74(H74A,H74B,
 H74C), C53(H53A,H53B,H53C), C111(H11M,H11N,H11O), C110(H11P,H11Q,H11R),
 C85(H85A,H85B,H85C), C63(H63A,H63B,H63C), C16(H16A,H16B,H16C), C41(H41A,H41B,
 H41C), C29(H29A,H29B,H29C), C119(H11U,H11V,H11W)
;
_shelx_res_checksum              12145
_shelx_hkl_checksum              20752
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'