Mononuclear Fe(I) and Fe(II) Acetylene Adducts and Their Reductive Protonation to Terminal Fe(IV) and Fe(V) Carbynes.
Citek, Cooper; Oyala, Paul H.; Peters, Jonas C.; Journal of the American Chemical Society 141 (2019) 15211–15221; doi:10.1021/jacs.9b06987

data_4128992
_publ_section_title
;
 Mononuclear Fe(I) and Fe(II) Acetylene Adducts and Their Reductive
 Protonation to Terminal Fe(IV) and Fe(V) Carbynes.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15211
_journal_page_last               15221
_journal_paper_doi               10.1021/jacs.9b06987
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C37.83 H56.75 Cl0.08 Fe P3 Si'
_chemical_formula_sum            'C37.83 H56.75 Cl0.08 Fe P3 Si'
_chemical_formula_weight         691.34
_chemical_name_systematic        SiP3FeCCH3
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.999(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2971(8)
_cell_length_b                   16.1450(9)
_cell_length_c                   17.0059(10)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.22
_cell_measurement_theta_min      2.80
_cell_volume                     3645.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            161412
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.567
_diffrn_reflns_theta_min         2.794
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0902 before and 0.0522 after correction. The Ratio of minimum to maximum transmission is 0.9477. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1481
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         19652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16929
_reflns_number_total             19652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06987_si_002.cif
_cod_data_source_block           p17673
_cod_database_code               4128992
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C6)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C40(H40), C25(H25), C14(H14), C28(H28), C37(H37)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C11(H11), C12(H12), C36(H36), C35(H35), C24(H24), C13(H13),
 C23(H23), C34(H34), C10(H10), C33(H33), C22(H22)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C15(H15A,H15B,H15C), C42(H42A,
 H42B,H42C), C26(H26A,H26B,H26C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C),
 C00Q(H00A,H00B,H00C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              86416
_shelx_hkl_checksum              41419
_olex2_submission_special_instructions 'No special instructions were received'