Imine-Centered Reactions in Imino-Phosphine Complexes of Iron Carbonyls
Chu, Wan-Yi; Richers, Casseday P.; Kahle, Elizabeth R.; Rauchfuss, Thomas B.; Arrigoni, Federica; Zampella, Giuseppe; Organometallics 35 (2016) 2782–; doi:10.1021/acs.organomet.6b00318

data_4086657
_publ_section_title
;
 Imine-Centered Reactions in Imino-Phosphine Complexes of Iron Carbonyls
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2782
_journal_paper_doi               10.1021/acs.organomet.6b00318
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H38 Cl2 Fe N2 O2 P2'
_chemical_formula_sum            'C52 H38 Cl2 Fe N2 O2 P2'
_chemical_formula_weight         911.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5666(8)
_cell_length_b                   11.3932(4)
_cell_length_c                   40.4725(14)
_cell_measurement_reflns_used    7980
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      66.49
_cell_measurement_theta_min      3.92
_cell_volume                     10400.3(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      183.15
_diffrn_detector                 'Bruker APEXII CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            48336
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.635
_diffrn_reflns_theta_min         3.920
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Siemens fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.146
_exptl_absorpt_correction_T_max  0.6350
_exptl_absorpt_correction_T_min  0.1732
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0882 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.2728.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       prism
_exptl_crystal_F_000             3760
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 0 0) scattering 
planes roughly normal to the spindle axis.  
;
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0493P)^2^+7.9767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6761
_reflns_number_total             8994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00318_si_003.cif
_cod_data_source_block           FeP2N2
_cod_depositor_comments
'Adding full bibliography for 4086653--4086659.cif.'
_cod_database_code               4086657
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.255
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_smtbx_masks_special_details
;
The electron density map suggested the presence of 2 CH2Cl2 and 1/2 pentane
per molecule of FeP2N2(CO)2. The total number of electrons masked were 866,
correpsonding to 16 CH2Cl2 and 4 pentanes. Given Z = 8, this is roughly
consistent with 2 CH2Cl2 and 1/2 pentane per molecule.
;
_shelx_res_checksum              20049
_shelx_hkl_checksum              29026
_olex2_submission_special_instructions 'No special instructions were received'