Structural and Electronic Variations of sp/sp2Carbon-Based Bridges in Di- and Trinuclear Redox-Active Iron Complexes Bearing Fe(diphosphine)2X (X = I, NCS) Moieties
Lissel, Franziska; Blacque, Olivier; Venkatesan, Koushik; Berke, Heinz; Organometallics 34 (2015) 408–; doi:10.1021/om500602m

data_4085282
_publ_section_title
;
 Structural and Electronic Variations of sp/sp2Carbon-Based Bridges in Di-
 and Trinuclear Redox-Active Iron Complexes Bearing Fe(diphosphine)2X (X =
 I, NCS) Moieties
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              408
_journal_paper_doi               10.1021/om500602m
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C72 H147 Fe3 I3 P12, 0.5(C6 H6)'
_chemical_formula_sum            'C75 H150 Fe3 I3 P12'
_chemical_formula_weight         1971.83
_chemical_name_systematic
(\m^3^-1,3,5-Benzenetriethynyl)-hexakis(ethane-1,2-diylbis(diethylphosphine))-triiodo-triiron
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.221(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5273(5)
_cell_length_b                   28.5966(10)
_cell_length_c                   20.0805(7)
_cell_measurement_reflns_used    8211
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.7132
_cell_measurement_theta_min      2.2412
_cell_volume                     9309.1(6)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.36.32 (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae et al., 2006)
;
_computing_publication_material
; 
Olex2 (Dolomanov et al., 2009), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0408116000
_diffrn_orient_matrix_UB_12      0.0469254000
_diffrn_orient_matrix_UB_13      0.0249637000
_diffrn_orient_matrix_UB_21      -0.0730471000
_diffrn_orient_matrix_UB_22      0.0114506000
_diffrn_orient_matrix_UB_23      0.0345917000
_diffrn_orient_matrix_UB_31      0.0450744000
_diffrn_orient_matrix_UB_32      -0.0238571000
_diffrn_orient_matrix_UB_33      0.0655430000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1258
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50707
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.729
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             4068
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.537
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         17043
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.2208
_refine_ls_R_factor_gt           0.1298
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3467
_refine_ls_wR_factor_ref         0.4288
_reflns_number_gt                7144
_reflns_number_total             17043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500602m_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085279--4085285.cif.'
_cod_database_code               4085282
_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. Restrained distances
 C13-C14
 1.52 with sigma of 0.01
 C17-C18
 1.52 with sigma of 0.01
 C27-C28
 1.52 with sigma of 0.01
 C31-C32
 1.52 with sigma of 0.01
 C33-C34
 1.52 with sigma of 0.01
 C37-C38
 1.52 with sigma of 0.01
 C43-C44
 1.52 with sigma of 0.01
 C45-C46
 1.52 with sigma of 0.01
 C49-C50
 1.52 with sigma of 0.01
 C53-C54
 1.52 with sigma of 0.01
 C57-C58
 1.52 with sigma of 0.01
 C61-C62
 1.52 with sigma of 0.01
 C59-C60
 1.52 with sigma of 0.01
 C63-C64
 1.52 with sigma of 0.01
 C67-C68
 1.52 with sigma of 0.01
 C69-C70 = C71-C72
 1.52 with sigma of 0.01
 C73-C74 = C74-C75 = C75-C76 = C76-C77 = C77-C78 = C78-C73
 1.39 with sigma of 0.005
 C73-C75 = C74-C76 = C75-C77 = C76-C78 = C77-C73
 2.4 with sigma of 0.005
 C33-C37
 2.8 with sigma of 0.01
 C13-C17
 2.8 with sigma of 0.01
 C54-C60
 3.2 with sigma of 0.01
 P8-C49 \\sim P8-C51
 with sigma of 0.005
 P9-C53 \\sim P10-C54
 with sigma of 0.005
 Fe1-I1A \\sim Fe1-I1B
 with sigma of 0.005
 Fe2-I2A \\sim Fe2-I2B
 with sigma of 0.005
3. Restrained planarity
 C73, C74, C75, C76, C77, C78
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 4A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(I2A) = Uanis(I2B)
Uiso(C73) = Uiso(C74) = Uiso(C75) = Uiso(C76) = Uiso(C77) = Uiso(C78)
5. Others
 Fixed Sof: C73(0.5) H73(0.5) C74(0.5) H74(0.5) C75(0.5) H75(0.5) C76(0.5)
 H76(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) I3A(0.5) I3B(0.5) I2B(0.5)
 I2A(0.5) I1B(0.5) I1A(0.5)
 Fixed U11: Fe1(0.034562) Fe2(0.034931) Fe3(0.026875) P1(0.039294)
 P2(0.038315) P3(0.047151) P4(0.042887) P5(0.065682) P6(0.044068) P7(0.04463)
 P8(0.04824) P9(0.060146) P10(0.047614) P11(0.086351) P12(0.046348)
 C1(0.029477) C2(0.031408) C3(0.05824) C4(0.042685) C5(0.04859) C6(0.035802)
 C7(0.031915) C8(0.047412) C9(0.030646) C10(0.046052) C11(0.036454)
 C12(0.034515)
 Fixed U12: Fe1(0.002411) Fe2(-0.006769) Fe3(0.001371) P1(0.00238)
 P2(0.001275) P3(-0.00099) P4(-0.020751) P5(0.002204) P6(-0.003109)
 P7(0.008835) P8(0.000804) P9(0.005032) P10(0.001837) P11(0.028252) P12(-
 0.005888) C1(-0.009321) C2(0.019207) C3(-0.004093) C4(-0.014687) C5(0.005694)
 C6(-0.015303) C7(-0.016691) C8(0.018504) C9(-0.004461) C10(-0.001092) C11(-
 0.012865) C12(0.008865)
 Fixed U13: Fe1(0.002126) Fe2(-0.004298) Fe3(0.001757) P1(-0.010934)
 P2(0.00984) P3(-0.009527) P4(0.006767) P5(0.01598) P6(-0.015969) P7(0.015393)
 P8(-0.016233) P9(0.025229) P10(-0.006117) P11(0.010378) P12(0.003158) C1(-
 0.001116) C2(0.003704) C3(-0.016095) C4(0.007252) C5(-0.015842) C6(0.008961)
 C7(-0.00666) C8(0.014695) C9(0.005577) C10(-0.013587) C11(-0.011509)
 C12(0.001235)
 Fixed U22: Fe1(0.04547) Fe2(0.04687) Fe3(0.04416) P1(0.05462) P2(0.0745)
 P3(0.07697) P4(0.07858) P5(0.06251) P6(0.05004) P7(0.08496) P8(0.11128)
 P9(0.06477) P10(0.0458) P11(0.07921) P12(0.05417) C1(0.05888) C2(0.07715)
 C3(0.00796) C4(0.07846) C5(0.03222) C6(0.06411) C7(0.08752) C8(0.02836)
 C9(0.03826) C10(0.03997) C11(0.03988) C12(0.01966)
 Fixed U23: Fe1(0.00121) Fe2(0.00164) Fe3(-0.00763) P1(0.01154) P2(0.0075) P3(-
 0.00791) P4(0.01441) P5(-0.01327) P6(0.0074) P7(-0.00219) P8(0.01861)
 P9(0.027) P10(-0.0107) P11(0.01618) P12(-0.01652) C1(0.01692) C2(-0.00375) C3(-
 0.00342) C4(0.00101) C5(-0.00085) C6(0.00612) C7(-0.00708) C8(0.00524) C9(-
 0.01179) C10(-0.03237) C11(0.01233) C12(0.00501)
 Fixed U33: Fe1(0.08569) Fe2(0.08667) Fe3(0.08719) P1(0.08867) P2(0.08396)
 P3(0.10013) P4(0.09621) P5(0.1063) P6(0.1214) P7(0.08778) P8(0.10202)
 P9(0.14339) P10(0.08171) P11(0.08099) P12(0.09061) C1(0.07012) C2(0.06093)
 C3(0.07604) C4(0.0653) C5(0.08525) C6(0.07323) C7(0.07278) C8(0.07033)
 C9(0.10288) C10(0.10744) C11(0.0927) C12(0.08134)
 Fixed Uiso: C13(0.08) C14(0.08) C15(0.1) C16(0.15) C17(0.1) C18(0.15)
 C19(0.1) C20(0.15) C21(0.1) C22(0.15) C23(0.08) C24(0.08) C25(0.1) C26(0.15)
 C27(0.1) C28(0.15) C29(0.1) C30(0.15) C31(0.1) C32(0.15) C33(0.08) C34(0.08)
 C35(0.1) C36(0.15) C37(0.1) C38(0.15) C39(0.1) C40(0.15) C41(0.1) C42(0.15)
 C43(0.08) C44(0.08) C45(0.1) C46(0.15) C47(0.1) C48(0.15) C49(0.1) C50(0.15)
 C51(0.1) C52(0.15) C53(0.08) C54(0.08) C55(0.1) C56(0.15) C57(0.1) C58(0.15)
 C59(0.1) C60(0.15) C61(0.1) C62(0.15) C63(0.08) C64(0.08) C65(0.1) C66(0.15)
 C67(0.1) C68(0.15) C69(0.1) C70(0.15) C71(0.1) C72(0.15)
 Fixed X: C15(0.8598) C16(0.9331) C17(0.9602) C19(0.8241) C20(0.8899)
 C21(0.851001) C22(0.9414) C23(0.57) C24(0.598001) C25(0.657901) C26(0.577399)
 C27(0.624701) C29(0.7294) C30(0.6667) C31(0.660701) C37(0.88242) C39(0.8734)
 C40(0.931399) C41(0.951301) C42(1.036599) C45(0.6941) C47(0.7658) C48(0.7057)
 C51(0.665901) C52(0.5832) C55(0.1825) C56(0.2005) C57(0.351801) C59(0.3437)
 C61(0.193001) C65(0.157701) C66(0.1327) C67(0.2922) C69(0.279599) C71(0.164101)
 Fixed Y: C15(0.169901) C16(0.2034) C17(0.0869) C19(0.177) C20(0.199901)
 C21(0.0797) C22(0.0817) C23(0.0792) C24(0.0506) C25(0.0234) C26(0.009399)
 C27(0.122101) C29(0.0333) C30(0.0085) C31(0.125501) C37(0.472049) C39(0.3806)
 C40(0.341301) C41(0.4697) C42(0.4516) C45(0.428) C47(0.516) C48(0.5407)
 C51(0.5306) C52(0.5421) C55(0.1835) C56(0.155901) C57(0.188001) C59(0.3807)
 C61(0.361101) C65(0.3895) C66(0.4231) C67(0.3494) C69(0.2198) C71(0.1709)
 Fixed Z: C15(0.874599) C16(0.9105) C17(0.869301) C19(0.622201) C20(0.585999)
 C21(0.5836) C22(0.5707) C23(0.7028) C24(0.7708) C25(0.613201) C26(0.5737)
 C27(0.5904) C29(0.8793) C30(0.9126) C31(0.869901) C37(0.60589) C39(0.8729)
 C40(0.8747) C41(0.881801) C42(0.917) C45(0.8885) C47(0.9016) C48(0.9416)
 C51(0.617101) C52(0.5732) C55(0.8127) C56(0.882) C57(0.8029) C59(0.7809)
 C61(0.8323) C65(0.648201) C66(0.5871) C67(0.5831) C69(0.5656) C71(0.6361)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B), C49(H49A,H49B),
 C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B),
  C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C72(H72A,H72B,H72C)
;
_shelx_hkl_checksum              14911