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_7125184
_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         'C59 H88 N5 O Sm'
_chemical_formula_sum            'C59 H88 N5 O Sm'
_chemical_formula_weight         1033.69
_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                76.406(10)
_cell_angle_beta                 80.735(12)
_cell_angle_gamma                63.678(9)
_cell_formula_units_Z            2
_cell_length_a                   12.769(2)
_cell_length_b                   13.1625(14)
_cell_length_c                   20.932(3)
_cell_measurement_reflns_used    16787
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      1.75
_cell_volume                     3058.5(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.961
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.1012
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22795
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.130
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.9268
_exptl_absorpt_correction_T_min  0.8122
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRED & XSHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       plate
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.536
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         11699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8193
_reflns_number_total             11699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07367k2.cif
_cod_data_source_block           3
_cod_original_cell_volume        3058.4(8)
_cod_database_code               7125184
_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:
 C17(H17), C20(H20), C29(H29), C32(H32), C42(H42), C45(H45), C54(H54), C57(H57)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15), C25(H25), C26(H26), C27(H27),
 C35(H35), C38(H38), C39(H39), C40(H40), C50(H50), C51(H51), C52(H52)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C)
;
_shelx_res_checksum              31924
_shelx_hkl_checksum              9901
_shelx_fab_checksum              14350
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'