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_7048546
_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(C56 H138 Fe2 K2 N4 O12 Si8)'
_chemical_formula_sum            'C28 H69 Fe K N2 O6 Si4'
_chemical_formula_weight         737.16
_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   mixed
_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                94.5940(10)
_cell_angle_beta                 96.9240(10)
_cell_angle_gamma                96.112(2)
_cell_formula_units_Z            4
_cell_length_a                   9.1092(4)
_cell_length_b                   19.7540(9)
_cell_length_c                   23.9066(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.33
_cell_volume                     4227.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            126701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.806
_diffrn_reflns_theta_min         2.178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1094 before and 0.0547 after correction. The Ratio of minimum to maximum transmission is 0.9348. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       plank
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         18048
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0270P)^2^+2.6996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14223
_reflns_number_total             18048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05002c2.cif
_cod_data_source_block           k(18c6)_fenbu(5)
_cod_depositor_comments
'Adding full bibliography for 7048542--7048549.cif.'
_cod_database_code               7048546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.783
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C3 \\sim C0AA \\sim C2A \\sim C4: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C3) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C3, C0AA, C2A, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H3CG(0.25) H3CF(0.25) H3AC(0.5) H3AB(0.5) H3BD(0.25) H3BE(0.25)
 C0AA(0.5) H0AB(0.5) H0AC(0.5) H0AD(0.5) C2A(0.25) H2AB(0.25) H2AC(0.25)
 H2AD(0.25) C4(0.25) H4A(0.25) H4B(0.25) H4C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C1(H1A,H1B), C00V(H00A,H00B), C00X(H00F,H00G), C00Y(H00H,H00I),
 C00Z(H00J,H00K), C013(H01J,H01K), C016(H01R,H01S), C019(H01Z,H), C7(H7A,H7B),
 C01B(H01,HA), C01C(H0AA,HB), C01D(H1AA,HC), C01F(H3AA,HF), C01H(H5AA,HI),
 C01J(H7AA,HL), C6(H6A,H6B), C01M(H9AA,HO), C01N(H0BA,HP), C01O(H1BA,HQ),
 C01R(H3BA,HT), C01T(H5BA,HW), C01U(H6BA,HX), C01W(H8BA,H1CA), C01X(H9BA,H2CA),
 C021(H02D,H02E), C022(H02F,H02G), C2(H2A,H2B), C3(H3CG,H3CF), C3(H3AC,H3AB),
 C3(H3BD,H3BE)
5.b Idealised Me refined as rotating group:
 C00W(H00C,H00D,H00E), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,
 H01H,H01I), C014(H01L,H01M,H01N), C015(H01O,H01P,H01Q), C017(H01T,H01U,H01V),
 C018(H01W,H01X,H01Y), C01E(H2AA,HD,HE), C01G(H4AA,HG,HH), C01I(H6AA,HJ,HK),
 C01K(H8AA,HM,HN), C1AA(H1AB,H1AC,H1AD), C01Q(H2BA,HR,HS), C01S(H4BA,HU,HV),
 C01V(H7BA,HY,HZ), C8(H8A,H8B,H8C), C01Z(H0CA,H3CA,H4CA), C020(H02A,H02B,H02C),
 C023(H02H,H02I,H02J), C025(H02M,H02N,H02O), C026(H02P,H02Q,H02R), C027(H02S,
 H02T,H02U), C029(H02V,H02W,H02X), C02A(H02Y,H5CA,H6CA), C0AA(H0AB,H0AC,H0AD),
 C2A(H2AB,H2AC,H2AD), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              28757
_olex2_submission_special_instructions 'No special instructions were received'