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_7125185
_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 As5 Fe N8 O2 Sm2, C7 H16'
_chemical_formula_sum            'C125 H187 As5 Fe N8 O2 Sm2'
_chemical_formula_weight         2564.96
_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                108.733(4)
_cell_angle_beta                 93.697(5)
_cell_angle_gamma                93.654(5)
_cell_formula_units_Z            2
_cell_length_a                   13.1985(10)
_cell_length_b                   20.5277(9)
_cell_length_c                   24.6698(12)
_cell_measurement_reflns_used    24720
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.55
_cell_volume                     6291.4(7)
_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      150
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43132
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.382
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         1.573
_exptl_absorpt_coefficient_mu    2.389
_exptl_absorpt_correction_T_max  0.8740
_exptl_absorpt_correction_T_min  0.6119
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRED & XShape'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       needle
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1327
_refine_ls_number_reflns         22528
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13905
_reflns_number_total             22528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07367k2.cif
_cod_data_source_block           2
_cod_original_cell_volume        6291.4(6)
_cod_database_code               7125185
_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. Uiso/Uaniso restraints and constraints
O1 \\sim C1 \\sim C2: within 2A with sigma of 0.0008 and sigma for terminal
atoms of 0.0016
C37 \\sim C38 \\sim C39: within 2A with sigma of 0.008 and sigma for terminal
atoms of 0.016
C22 \\sim C23 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C34(H34), C37(H37), C47(H47), C50(H50), C59(H59),
 C62(H62), C72(H72), C75(H75), C84(H84), C87(H87), C97(H97), C100(H100),
 C109(H109), C112(H112)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C115(H11P,H11Q),
 C116(H11R,H11S), C117(H11T,H11U), C118(H11V,H11W), C120(H12D,H12E), C121(H12F,
 H12G), C122(H12H,H12I), C123(H12J,H12K), C124(H12L,H12M)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32),
 C40(H40), C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57), C65(H65),
  C68(H68), C69(H69), C70(H70), C80(H80), C81(H81), C82(H82), C90(H90),
 C93(H93), C94(H94), C95(H95), C105(H105), C106(H106), C107(H107)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C98(H98A,
 H98B,H98C), C99(H99A,H99B,H99C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I),
 C110(H11D,H11E,H11F), C111(H11G,H11H,H11I), C113(H11J,H11K,H11L), C114(H11M,
 H11N,H11O), C119(H11X,H11Y,H), C125(H12N,H12O,H12P)
;
_shelx_res_checksum              4966
_shelx_hkl_checksum              84896
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'