Mono- and dinuclear tetraphosphabutadiene ferrate anions.
Chakraborty, Uttam; Leitl, Julia; Mühldorf, Bernd; Bodensteiner, Michael; Pelties, Stefan; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3693–3697; doi:10.1039/c7dt04641c

data_7045634
_publ_section_title
;
 Mono- and dinuclear tetraphosphabutadiene ferrate anions.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3693
_journal_page_last               3697
_journal_paper_doi               10.1039/c7dt04641c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
;
C101.68 H110.93 Fe2 Na O2.81 P4, 
0.2 thf, 0.8 hexane
;
_chemical_formula_sum            'C101.69 H110.94 Fe2 Na O2.81 P4'
_chemical_formula_weight         1636.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-07
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5467)
;
_audit_update_record
;
2018-02-07 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4789(3)
_cell_length_b                   24.3950(2)
_cell_length_c                   16.5309(2)
_cell_measurement_reflns_used    28597
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3520
_cell_measurement_theta_min      3.7020
_cell_volume                     9468.37(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;

List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -125.00 -79.00   1.00    5.00    --  -43.98 -99.00-180.00   46
  2  \w    -97.00  -2.00   1.00    5.00    --  -43.98 125.00-180.00   95
  3  \w    -28.00  68.00   1.00    5.00    --   43.98 -37.00-180.00   96
  4  \w     34.00 129.00   1.00   20.00    --  104.50 -45.00-120.00   95
  5  \w     21.00 109.00   1.00   20.00    --  104.50 -94.00 -90.00   88
  6  \w     73.00 178.00   1.00   20.00    --  104.50 125.00 -90.00  105
  7  \w     80.00 175.00   1.00   20.00    --  104.50  45.00-120.00   95
  8  \w   -114.00 -18.00   1.00    5.00    --  -43.98 -57.00 -60.00   96
  9  \w   -114.00 -18.00   1.00    5.00    --  -43.98 -57.00-180.00   96
 10  \w     65.00 178.00   1.00   20.00    --  104.50  15.00  60.00  113
 11  \w     80.00 175.00   1.00   20.00    --  104.50  45.00 120.00   95
 12  \w     73.00 178.00   1.00   20.00    --  104.50  77.00 -30.00  105
 13  \w     73.00 178.00   1.00   20.00    --  104.50  77.00-180.00  105
 14  \w   -118.00 -12.00   1.00    5.00    --  -43.98 -77.00  60.00  106
 15  \w     73.00 118.00   1.00    5.00    --   43.98 125.00-180.00   45
 16  \w     30.00 136.00   1.00   20.00    --  104.50 -77.00   0.00  106
 17  \w     78.00 174.00   1.00   20.00    --  104.50  61.00 150.00   96
 18  \w     73.00 137.00   1.00   20.00    --  104.50  77.00  60.00   64
 19  \w     78.00 174.00   1.00   20.00    --  104.50  61.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517312000
_diffrn_orient_matrix_UB_12      0.0222418000
_diffrn_orient_matrix_UB_13      -0.0470505000
_diffrn_orient_matrix_UB_21      -0.0241363000
_diffrn_orient_matrix_UB_22      0.0585241000
_diffrn_orient_matrix_UB_23      0.0067660000
_diffrn_orient_matrix_UB_31      0.0324415000
_diffrn_orient_matrix_UB_32      0.0081225000
_diffrn_orient_matrix_UB_33      0.0801129000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            108153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.505
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             3466
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         9716
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0836
_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^)+(0.1575P)^2^+15.0112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2624
_refine_ls_wR_factor_ref         0.2756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7926
_reflns_number_total             9716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04641c2.cif
_cod_data_source_block           4mb
_cod_depositor_comments
'Adding full bibliography for 7045632--7045634.cif.'
_cod_database_code               7045634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.500
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C66-C65 = C65-C64 = C9-C10
 1.54 with sigma of 0.01
 O5-C70 \\sim O5-C67
 with sigma of 0.02
 C67-C68 \\sim C68-C69 \\sim C70-C69
 with sigma of 0.02
 C66-C65 \\sim C65-C64
 with sigma of 0.01
 C22-C20 \\sim C21-C20 \\sim C35-C27 \\sim C34-C27 \\sim C45-C44 \\sim C46-C44
\\sim C9-C10 \\sim C55-C53
 \\sim C54-C53
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C29 \\sim C32 \\sim C33 \\sim C28 \\sim C27 \\sim C35 \\sim
C34 \\sim C23 \\sim C25 \\sim C26 \\sim C36 \\sim C37 \\sim C24: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
P1 \\sim P3 \\sim P2 \\sim P4 \\sim P5 \\sim P6 \\sim P7: within 2.5A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim C59 \\sim C58 \\sim C57 \\sim C56: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.005
C54 \\sim C53 \\sim C55: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
C70 \\sim C69 \\sim C68 \\sim C67 \\sim O5: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.005
O3 \\sim C64 \\sim C65 \\sim C66 \\sim O4: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C21 \\sim C20 \\sim C22: within 1.9A with sigma of 0.001 and sigma for terminal
atoms of 0.001
4. Others
 Sof(H44C)=Sof(H44D)=Sof(H27C)=Sof(H27D)=Sof(H53C)=Sof(H53D)=Sof(H20C)=
 Sof(H20D)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(C36)=
 Sof(H36)=Sof(C37)=Sof(H37)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(1)
 Sof(P5)=Sof(P6)=Sof(P7)=0.5*(1-FVAR(2))
 Sof(P3)=Sof(P2)=Sof(P4)=0.5*FVAR(2)
 Sof(C30)=Sof(H30)=Sof(C31)=Sof(C29)=Sof(H29)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C28)=Sof(H44A)=Sof(H44B)=Sof(H27A)=Sof(H27B)=Sof(H53A)=Sof(H53B)=
 Sof(H20A)=Sof(H20B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(H65A)=Sof(H65B)=1-FVAR(2)
 Sof(Na2)=Sof(O4)=Sof(O5)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=0.5*(1-FVAR(3))
 Sof(Na1)=Sof(O1)=Sof(O3)=Sof(O2)=Sof(H18)=Sof(C62)=Sof(H62A)=Sof(H62B)=
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C61)=Sof(H61A)=
 Sof(H61B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C56)=
 Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C64)=Sof(H64A)=Sof(H64B)=
 0.5*FVAR(3)
 Fixed Sof: C69(0.5) H69A(0.5) H69B(0.5) C68(0.5) H68A(0.5) H68B(0.5) C67(0.5)
 H67A(0.5) H67B(0.5) C65(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C44(H44C,H44D), C9(H9A,H9B), C27(H27A,H27B), C27(H27C,H27D),
 C53(H53A,H53B), C53(H53C,H53D), C20(H20A,H20B), C20(H20C,H20D), C62(H62A,H62B),
  C58(H58A,H58B), C63(H63A,H63B), C61(H61A,H61B), C60(H60A,H60B), C59(H59A,
 H59B), C56(H56A,H56B), C57(H57A,H57B), C69(H69A,H69B), C68(H68A,H68B),
 C67(H67A,H67B), C70(H70A,H70B), C65(H65A,H65B), C64(H64A,H64B), C66(H66A,H66B)
5.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C), C35(H35A,H35B,
 H35C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C46(H46A,
 H46B,H46C), C55(H55A,H55B,H55C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C48(H48), C30(H30), C52(H52), C39(H39), C8(H8), C49(H49), C51(H51),
 C40(H40), C5(H5), C7(H7), C43(H43), C15(H15), C29(H29), C32(H32), C42(H42),
 C33(H33), C19(H19), C16(H16), C18(H18), C24(H24), C25(H25), C36(H36), C37(H37)
5.d Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C36,C37)
;
_shelx_res_checksum              71233
_shelx_fab_checksum              43226
_olex2_submission_special_instructions 'No special instructions were received'