Proton reduction by phosphinidene-capped triiron clusters
Rahaman, Ahibur; Lisensky, George C.; Haukka, Matti; Tocher, Derek A.; Richmond, Michael G.; Colbran, Stephen B.; Nordlander, Ebbe; Journal of Organometallic Chemistry 943 (2021) 121816–; doi:10.1016/j.jorganchem.2021.121816

data_4038978
_publ_section_title
;
 Proton reduction by phosphinidene-capped triiron clusters
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              121816
_journal_paper_doi               10.1016/j.jorganchem.2021.121816
_journal_volume                  943
_journal_year                    2021
_chemical_formula_moiety         'C53 H38 Fe4 O7 P4, C H2 Cl2'
_chemical_formula_sum            'C54 H40 Cl2 Fe4 O7 P4'
_chemical_formula_weight         1219.04
_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     iterative
_cell_angle_alpha                90
_cell_angle_beta                 96.8651(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.13225(4)
_cell_length_b                   20.92716(9)
_cell_length_c                   21.95729(9)
_cell_measurement_reflns_used    51565
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3250
_cell_measurement_theta_min      4.2040
_cell_volume                     5078.64(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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omega____ theta____ kappa____ phi______ frames
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  2 omega   23.00   88.00   1.0000    2.0950
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  3 omega   24.00  106.00   1.0000    8.3850
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  4 omega   67.00  107.00   1.0000    8.3850
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  5 omega   35.00  134.00   1.0000    8.3850
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  6 omega   77.00  103.00   1.0000    8.3850
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  7 omega  105.00  134.00   1.0000    8.3850
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  8 omega  140.00  167.00   1.0000    8.3850
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  9 omega   76.00  101.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 10 omega   77.00  165.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 11 omega   74.00  165.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 12 omega   77.00  174.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 13 omega   75.00  101.00   1.0000    8.3850
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 14 omega   76.00  118.00   1.0000    8.3850
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 15 omega   77.00  103.00   1.0000    8.3850
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 16 omega   77.00  105.00   1.0000    8.3850
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 17 omega   77.00  163.00   1.0000    8.3850
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 18 omega   77.00  103.00   1.0000    8.3850
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 19 omega   77.00  103.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 20 omega   74.00  142.00   1.0000    8.3850
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 21 omega   76.00  173.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 22 omega   74.00  167.00   1.0000    8.3850
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 23 omega   77.00  104.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 24 omega   76.00  102.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 25 omega   74.00  100.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000    0.0000 26

 26 omega   74.00  178.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000  -30.0000 104

 27 omega   74.00   99.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000  -60.0000 25

 28 omega   76.00  102.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 29 omega   74.00  100.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000 -180.0000 26

 30 omega   25.00  109.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614  -94.0000   60.0000 84

 31 omega   33.00   97.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 32 omega   78.00  162.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 33 omega   77.00  102.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 34 omega   77.00  167.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 35 omega   77.00  103.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
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 36 omega   74.00  100.00   1.0000    8.3850
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    -      106.3614   77.0000  150.0000 26

 37 omega   74.00  100.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000  120.0000 26

 38 omega   77.00  103.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   61.0000   60.0000 26

 39 omega   34.00  121.00   1.0000    8.3850
omega____ theta____ kappa____ phi______ frames
    -      106.3614 -125.0000 -150.0000 87

 40 omega  -54.00  -10.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -77.0000   30.0000 44

 41 omega  -55.00  -14.00   1.0000    2.0950
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    -      -42.6216  -77.0000   90.0000 41

 42 omega  -55.00  -10.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -77.0000  150.0000 45

 43 omega  -58.00   -3.00   1.0000    2.0950
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 44 omega  -69.00  -18.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -38.0000    0.0000 51

 45 omega  -74.00   33.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216   77.0000 -150.0000 107

 46 omega -117.00  -86.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
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 47 omega -118.00  -78.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -77.0000  150.0000 40

 48 omega -118.00  -77.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
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 49 omega -114.00  -10.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
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 50 omega -119.00  -10.00   1.0000    2.0950
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -77.0000 -120.0000 109
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_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            86973
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.579
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
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_exptl_crystal_F_000             2472
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_exptl_crystal_size_mid          0.21
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_refine_diff_density_max         0.331
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_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0371P)^2^+5.0180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9843
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xstr0358.cif
_cod_data_source_block           xstr0358
_cod_database_code               4038978
_chemical_oxdiff_formula         'Fe3 P4 O7 C53 H38'
_chemical_oxdiff_usercomment     'AR 157B'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
;