C-Halide bond cleavage by a two-coordinate iron(i) complex.
Werncke, C. G.; Pfeiffer, J.; Müller, I; Vendier, L.; Sabo-Etienne, S; Bontemps, S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1757–1765; doi:10.1039/c8dt05002c

data_7048548
_publ_section_title
;
 C-Halide bond cleavage by a two-coordinate iron(i) complex.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1757
_journal_page_last               1765
_journal_paper_doi               10.1039/c8dt05002c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '1(C24 H60 Br2 Fe K N2 O6 Si4)'
_chemical_formula_sum            'C24 H60 Br2 Fe K N2 O6 Si4'
_chemical_formula_weight         839.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2018-11-08 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                111.8930(10)
_cell_angle_beta                 98.352(2)
_cell_angle_gamma                99.4360(10)
_cell_formula_units_Z            4
_cell_length_a                   12.1198(5)
_cell_length_b                   18.0228(7)
_cell_length_c                   20.7923(9)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.26
_cell_volume                     4050.1(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            131290
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction, wR2(int) was 0.1262 before and 0.0540 after correction. The Ratio of minimum to maximum transmission is 0.8543. The \I\2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         14259
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0286P)^2^+4.8751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12001
_reflns_number_total             14259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05002c2.cif
_cod_data_source_block           k(18c6)_febr2_(3a)
_cod_depositor_comments
'Adding full bibliography for 7048542--7048549.cif.'
_cod_database_code               7048548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.557
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br5-Fe2 \\sim Br4-Fe2
 with sigma of 0.02
 Si7-N3 \\sim Si8-N3
 with sigma of 0.02
 Si7-C17 \\sim Si8-C18
 with sigma of 0.02
 Si7-C15 \\sim Si8-C16
 with sigma of 0.02
 Si7-C13 \\sim Si8-C14
 with sigma of 0.02
 N3-C17 \\sim N3-C18
 with sigma of 0.04
 N3-C15 \\sim N3-C16
 with sigma of 0.04
 N3-C13 \\sim N3-C14
 with sigma of 0.04
 C17-C15 \\sim C18-C16
 with sigma of 0.04
 C17-C13 \\sim C18-C14
 with sigma of 0.04
 C15-C13 \\sim C16-C14
 with sigma of 0.04
 K1-O15 \\sim K1-O16
 with sigma of 0.02
 K1-O18 \\sim K1-O19
 with sigma of 0.02
 K1-O13 \\sim K1-O14
 with sigma of 0.02
 K1-O7 \\sim K1-O21
 with sigma of 0.02
 K1-O9 \\sim K1-O10
 with sigma of 0.02
 K1-O11 \\sim K1-O12
 with sigma of 0.02
 O15-C52 \\sim O16-C53
 with sigma of 0.02
 O15-C50 \\sim O16-C51
 with sigma of 0.02
 O18-C54 \\sim O19-C55
 with sigma of 0.02
 O18-C56 \\sim O19-C57
 with sigma of 0.02
 O13-C48 \\sim O14-C49
 with sigma of 0.02
 O13-C46 \\sim O14-C47
 with sigma of 0.02
 O7-C58 \\sim O21-C59
 with sigma of 0.02
 O7-C60 \\sim O21-C61
 with sigma of 0.02
 O9-C63 \\sim O10-C41
 with sigma of 0.02
 O9-C020 \\sim O10-C62
 with sigma of 0.02
 O11-C42 \\sim O12-C43
 with sigma of 0.02
 O11-C44 \\sim O12-C45
 with sigma of 0.02
 C52-C54 \\sim C53-C55
 with sigma of 0.02
 C56-C58 \\sim C57-C59
 with sigma of 0.02
 C50-C48 \\sim C51-C49
 with sigma of 0.02
 C63-C42 \\sim C41-C43
 with sigma of 0.02
 C020-C60 \\sim C62-C61
 with sigma of 0.02
 C46-C44 \\sim C47-C45
 with sigma of 0.02
 K1-C52 \\sim K1-C53
 with sigma of 0.04
 K1-C54 \\sim K1-C55
 with sigma of 0.04
 K1-C56 \\sim K1-C57
 with sigma of 0.04
 K1-C50 \\sim K1-C51
 with sigma of 0.04
 K1-C48 \\sim K1-C49
 with sigma of 0.04
 K1-C63 \\sim K1-C41
 with sigma of 0.04
 K1-C58 \\sim K1-C59
 with sigma of 0.04
 K1-C020 \\sim K1-C62
 with sigma of 0.04
 K1-C42 \\sim K1-C43
 with sigma of 0.04
 K1-C60 \\sim K1-C61
 with sigma of 0.04
 K1-C46 \\sim K1-C47
 with sigma of 0.04
 K1-C44 \\sim K1-C45
 with sigma of 0.04
 O15-C54 \\sim O16-C55
 with sigma of 0.04
 O15-C48 \\sim O16-C49
 with sigma of 0.04
 O18-C52 \\sim O19-C53
 with sigma of 0.04
 O18-C58 \\sim O19-C59
 with sigma of 0.04
 O13-C50 \\sim O14-C51
 with sigma of 0.04
 O13-C44 \\sim O14-C45
 with sigma of 0.04
 O7-C56 \\sim O21-C57
 with sigma of 0.04
 O7-C020 \\sim O21-C62
 with sigma of 0.04
 O9-C42 \\sim O10-C43
 with sigma of 0.04
 O9-C60 \\sim O10-C61
 with sigma of 0.04
 O11-C63 \\sim O12-C41
 with sigma of 0.04
 O11-C46 \\sim O12-C47
 with sigma of 0.04
 C52-C50 \\sim C53-C51
 with sigma of 0.04
 C54-C56 \\sim C55-C57
 with sigma of 0.04
 C48-C46 \\sim C49-C47
 with sigma of 0.04
 C63-C020 \\sim C41-C62
 with sigma of 0.04
 C58-C60 \\sim C59-C61
 with sigma of 0.04
 C42-C44 \\sim C43-C45
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C59) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C47)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(Si8)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(Si7)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(O10)=Sof(O12)=Sof(O14)=Sof(O16)=Sof(O19)=Sof(O21)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C57)=Sof(H57A)=
 Sof(H57B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=
 Sof(H62A)=Sof(H62B)=1-FVAR(2)
 Sof(O7)=Sof(O9)=Sof(O11)=Sof(O13)=Sof(O15)=Sof(O18)=Sof(C020)=Sof(H02A)=
 Sof(H02B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=FVAR(2)
 Fixed Sof: Br5(0.5) Br4(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C020(H02A,H02B), C42(H42A,H42B), C44(H44A,H44B), C46(H46A,H46B), C48(H48A,
 H48B), C50(H50A,H50B), C52(H52A,H52B), C54(H54A,H54B), C56(H56A,H56B),
 C58(H58A,H58B), C60(H60A,H60B), C63(H63A,H63B), C41(H41A,H41B), C43(H43A,H43B),
  C45(H45A,H45B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,
 H53B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B),
 C62(H62A,H62B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              26804
_olex2_submission_special_instructions 'No special instructions were received'