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_4038976
_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         'C49 H34 Fe3 O8 P4, C H2 Cl2'
_chemical_formula_sum            'C50 H36 Cl2 Fe3 O8 P4'
_chemical_formula_weight         1127.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                75.0870(10)
_cell_angle_beta                 81.1350(10)
_cell_angle_gamma                74.4750(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1306(2)
_cell_length_b                   12.3357(2)
_cell_length_c                   18.7045(3)
_cell_measurement_reflns_used    56326
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     2381.11(7)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2008)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'CrystaMaker X (CrystalMaker Software ltd., 2020)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41663
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.907
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.8388
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker, 2012)'
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11780
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+6.9011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9671
_reflns_number_total             11780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ar84a.cif
_cod_data_source_block           ar84a
_cod_database_code               4038976
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.774
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              11758
_shelx_hkl_checksum              23191