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_7045633
_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         'C110 H130 Fe2 Na2 O5 P4'
_chemical_formula_sum            'C110 H130 Fe2 Na2 O5 P4'
_chemical_formula_weight         1813.69
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-03
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5465)
;
_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                   23.2636(5)
_cell_length_b                   25.7313(5)
_cell_length_c                   16.0339(4)
_cell_measurement_reflns_used    21228
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      27.3890
_cell_measurement_theta_min      3.5060
_cell_volume                     9597.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.914
_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    -84.00 -58.00   1.00   90.00    --  -16.78 -77.00  60.00   26
  2  \w    -15.00  12.00   1.00   90.00    --  -16.78 -77.00  60.00   27
  3  \w    -79.00 -36.00   1.00   90.00    --  -16.78 -38.00-120.00   43
  4  \w    -56.00   4.00   1.00   90.00    --  -16.78 -38.00 -30.00   60
  5  \w    -30.00  -1.00   1.00   90.00    --  -16.78 -57.00-120.00   29
  6  \w    -95.00 -34.00   1.00   90.00    --  -16.78 178.00 150.00   61
  7  \w    -95.00 -70.00   1.00   90.00    --  -16.78-178.00  30.00   25
  8  \w    -38.00  52.00   1.00   90.00    --  -16.78  57.00  30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0291572000
_diffrn_orient_matrix_UB_12      -0.0035108000
_diffrn_orient_matrix_UB_13      -0.0116964000
_diffrn_orient_matrix_UB_21      0.0079428000
_diffrn_orient_matrix_UB_22      -0.0011810000
_diffrn_orient_matrix_UB_23      0.0426645000
_diffrn_orient_matrix_UB_31      -0.0040835000
_diffrn_orient_matrix_UB_32      -0.0273125000
_diffrn_orient_matrix_UB_33      -0.0002817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62104
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.033
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         10867
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+22.5744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9081
_reflns_number_total             10867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04641c2.cif
_cod_data_source_block           mb
_cod_depositor_comments
'Adding full bibliography for 7045632--7045634.cif.'
_cod_database_code               7045633
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C110H130Fe2P4Na2
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C13A-C12 = C13-C12
 1.54 with sigma of 0.01
 C36B-C33 \\sim C36A-C33
 with sigma of 0.02
 C37A-C36A \\sim C37B-C36B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C36B \\sim C36A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
4. Rigid body (RIGU) restrains
 C33, C36A, C36B, C37B, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C36A)=Sof(H36C)=Sof(H36D)=FVAR(1)
 Fixed Sof: C60B(0.5) H60A(0.5) H60B(0.5) H59A(0.5) H59B(0.5) H56A(0.5)
 H56B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C53(0.5) H53A(0.5) H53B(0.5) C54B(0.5)
 H54A(0.5) H54B(0.5) C46(0.5) H46A(0.5) H46B(0.5) C49(0.5) H49A(0.5) H49B(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C47B(0.5)
 H47A(0.5) H12A(0.55) H12B(0.55) H12C(0.45) H12D(0.45) C62(0.5) H62A(0.5)
 H62B(0.5) C13(0.55) H13A(0.55) H13B(0.55) H13C(0.55) C13A(0.45) H13D(0.45)
 H13E(0.45) H13F(0.45) C60A(0.5) H60C(0.5) H60D(0.5) C48A(0.5) H48A(0.5)
 H48B(0.5) C54A(0.5) H54C(0.5) H54D(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 C0AA(0.5) H0AA(0.5) H0AB(0.5)
6.a Riding coordinates:
 C60B(H60A,H60B), C59(H59A,H59B), C56(H56A,H56B), C61(H61A,H61B), C62(H62A,H62B)
6.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C53(H53A,H53B), C54B(H54A,H54B), C46(H46A,H46B), C49(H49A,
 H49B), C20(H20A,H20B), C58(H58A,H58B), C57(H57A,H57B), C44(H44A,H44B),
 C51(H51A,H51B), C52(H52A,H52B), C47B(H47A,H47B), C12(H12A,H12B), C12(H12C,
 H12D), C36B(H36A,H36B), C28(H28A,H28B), C60A(H60C,H60D), C48A(H48A,H48B),
 C54A(H54C,H54D), C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C36A(H36C,H36D)
6.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C31(H31), C35(H35), C15(H15), C19(H19), C23(H23), C27(H27),
 C43(H43), C39(H39), C16(H16), C40(H40), C8(H8), C10(H10), C32(H32), C34(H34),
 C18(H18), C24(H24), C26(H26), C42(H42)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C13A(H13D,H13E,H13F), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              89752
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.703