3d-4f heterometallic complexes by the reduction of transition metal carbonyls with bulky Ln<sup>II</sup> amidinates.
Yadav, Ravi; Hossain, Md Elius; Peedika Paramban, Ramees; Simler, Thomas; Schoo, Christoph; Wang, Jun; Deacon, Glen B.; Junk, Peter C.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7701–7707; doi:10.1039/d0dt01271h

data_7704379
_publ_section_title
;
 3d-4f heterometallic complexes by the reduction of transition metal
 carbonyls with bulky Ln<sup>II</sup> amidinates.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7701
_journal_page_last               7707
_journal_paper_doi               10.1039/d0dt01271h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C111 H140 Fe3 N8 O11 Sm2, 4(C7 H8)'
_chemical_formula_sum            'C139 H172 Fe3 N8 O11 Sm2'
_chemical_formula_weight         2599.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-30
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-04-03 deposited with the CCDC.	2020-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4276(4)
_cell_length_b                   20.8564(3)
_cell_length_c                   18.0530(4)
_cell_measurement_reflns_used    72953
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      1.95
_cell_volume                     6548.2(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
;
_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      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67255
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.614
_diffrn_reflns_theta_min         1.853
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.4439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE XRED, XSHAPE & LANA'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         15423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13087
_reflns_number_total             15423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01271h2.cif
_cod_data_source_block           ry235
_cod_depositor_comments
'Adding full bibliography for 7704376--7704379.cif.'
_cod_database_code               7704379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.681
_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. Others
 Fixed Sof: Fe1(0.5) Fe2(0.5) Fe3(0.5) H58A(0.5) H58(0.5) C0(0.5) O2(0.5)
 C2(0.5) O5(0.5) O6(0.5) C6(0.5) C8(0.5) O8(0.5) C9(0.5) O9(0.5) C59B(0.5)
 H59A(0.5) H59B(0.5) H59C(0.5) C60B(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C3(0.5)
 O3(0.5) O4(0.5) C5(0.5) O7(0.5) C7(0.5) O10(0.5) C10(0.5) C59A(0.5) H59D(0.5)
 H59E(0.5) H59F(0.5) C60A(0.5) H60D(0.5) H60E(0.5) H60F(0.5)
3.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33), C43(H43), C46(H46), C55(H55),
 C58(H58A), C58(H58)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28),
 C36(H36), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52), C53(H53), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71), C72(H72),
 C73(H73), C74(H74)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59B(H59A,H59B,
 H59C), C60B(H60A,H60B,H60C), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F),
 C61(H61A,H61B,H61C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              84285
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'