Homoleptic mono-, di-, and tetra-iron complexes featuring phosphido ligands: a synthetic, structural, and spectroscopic study.
Kaniewska, Kinga; Ponikiewski, Łukasz; Szynkiewicz, Natalia; Cieślik, Bartłomiej; Pikies, Jerzy; Krzystek, J.; Dragulescu-Andrasi, Alina; Stoian, Sebastian A.; Grubba, Rafał; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10091–10103; doi:10.1039/d0dt01503b

data_7704761
_publ_section_title
;
 Homoleptic mono-, di-, and tetra-iron complexes featuring phosphido
 ligands: a synthetic, structural, and spectroscopic study.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10091
_journal_page_last               10103
_journal_paper_doi               10.1039/d0dt01503b
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C60  H110  Fe2 P5, C12 H30 O6 Li1, C2 H5 O1'
_chemical_formula_sum            'C74 H145 Fe2 Li O7 P5'
_chemical_formula_weight         1420.38
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      34
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'iterative - e.g. charge flipping method'
_atom_sites_solution_secondary   'iterative - e.g. charge flipping method'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2020-05-24T18:52:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-06-02 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6571(2)
_cell_length_b                   25.8470(4)
_cell_length_c                   13.2128(6)
_cell_measurement_reflns_used    62460
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.70
_cell_measurement_wavelength     0.71073
_cell_volume                     8079.2(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017) 
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      ' 261 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            83344
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.306
_diffrn_reflns_theta_min         2.7
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 6486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     727
_refine_ls_number_reflns         21750
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.058
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+3.8660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.98
_reflns_number_gt                16759
_reflns_number_total             21750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01503b2.cif
_cod_data_source_block           kk48
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_radiation_monochromator' was replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 7550 2019-12-06 10:49:48Z antanas 

 Adding full bibliography for 7704757--7704761.cif.
;
_cod_database_code               7704761
_shelx_fab_checksum              38386