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_7048547
_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         '0.5(C62 H134 Fe2 K2 N4 O12 Si8)'
_chemical_formula_sum            'C31 H67 Fe K N2 O6 Si4'
_chemical_formula_weight         771.17
_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             2018-11-07
_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                91.857(4)
_cell_angle_beta                 94.986(4)
_cell_angle_gamma                92.202(4)
_cell_formula_units_Z            4
_cell_length_a                   9.0328(9)
_cell_length_b                   19.980(2)
_cell_length_c                   24.078(3)
_cell_measurement_reflns_used    6222
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.18
_cell_volume                     4323.1(8)
_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      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94329
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.183
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1387 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.9172.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.056
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         15131
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.1083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+93.8477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.2697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12676
_reflns_number_total             15131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05002c2.cif
_cod_data_source_block           k(18c6)_febz(2)
_cod_depositor_comments
'Adding full bibliography for 7048542--7048549.cif.'
_cod_original_cell_volume        4323.0(8)
_cod_database_code               7048547
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.757
_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
C9 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C8: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Si2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim C32 \\sim C35 \\sim C30 \\sim C31 \\sim C34: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Si2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C20) = Uanis(C11) = Uanis(C12) = Uanis(C10) = Uanis(C13) = Uanis(C14)
Uanis(C19) = Uanis(C16) = Uanis(C15) = Uanis(C8) = Uanis(C9) = Uanis(C18) =
Uanis(C17)
Uanis(C32) = Uanis(C31)
Uanis(C1) = Uanis(C3)
3. Rigid body (RIGU) restrains
 C9, C15, C16, C17, C18, C19, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C32, C35, C30, C31, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) C15(0.45) H15(0.45) C16(0.45) H16(0.45) C17(0.45)
 H17(0.45) C18(0.45) H18(0.45) C19(0.45) H19(0.45) C20(0.45) H20A(0.45)
 H20B(0.45) C8(0.55) H8A(0.55) H8B(0.55) C10(0.55) H10(0.55) C11(0.55)
 H11(0.55) C12(0.55) H12(0.55) C13(0.55) H13(0.55) C14(0.55) H14(0.55)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
  C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C20(H20A,H20B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
5.c Idealised Me refined as rotating group:
 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), C28(H28A,
 H28B,H28C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C29(H29A,H29B,H29C),
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              7759
_olex2_submission_special_instructions 'No special instructions were received'