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_7045632
_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         'C57 H69 Fe K O6 P4, C4 H10 O'
_chemical_formula_sum            'C61 H79 Fe K O7 P4'
_chemical_formula_weight         1143.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-12
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5433)
;
_audit_update_record
;
2018-01-12 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9516(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.36501(15)
_cell_length_b                   16.04859(13)
_cell_length_c                   22.20094(18)
_cell_measurement_reflns_used    21184
_cell_measurement_temperature    122.8(1)
_cell_measurement_theta_max      66.4930
_cell_measurement_theta_min      3.7620
_cell_volume                     6074.37(9)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      122.8(6)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44698
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.718
_diffrn_reflns_theta_min         3.420
_exptl_absorpt_coefficient_mu    3.989
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         10689
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0348P)^2^+2.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9843
_reflns_number_total             10689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04641c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045632--7045634.cif.'
_cod_original_cell_volume        6074.36(9)
_cod_database_code               7045632
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3AA-C1A \\sim C2AA-C1A \\sim C3AA-C19 \\sim C2AA-C15 \\sim C16-C15 \\sim
C17-C16 \\sim C17-C18 \\sim C18-
 C19
 with sigma of 0.02
3. Restrained planarity
 C14, C15, C16, C17, C18, C19
 with sigma of 0.1
 C1A, C2AA, C3AA, C14, C15, C19
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2AA \\sim C3AA \\sim C16 \\sim C18: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
5. Others
 Sof(C3AA)=Sof(H3AA)=Sof(H19A)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(H19)=FVAR(1)
 Fixed Sof: C1A(0.5) C2AA(0.5) H2AA(0.5) H15(0.5) H15A(0.5) C16(0.5) H16(0.5)
 C17(0.5) C20(0.5) H20A(0.5) H20B(0.5) C20A(0.5) H20C(0.5) H20D(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C20(H20A,H20B), C20A(H20C,H20D), C28(H28A,H28B), C36(H36A,
 H36B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
6.b Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C3AA(H3AA), C7(H7), C8(H8), C10(H10), C11(H11), C15(H15),
 C15(H15A), C16(H16), C18(H18), C19(H19), C19(H19A), C23(H23), C24(H24),
 C26(H26), C27(H27), C31(H31), C32(H32), C34(H34), C35(H35), C39(H39), C40(H40),
  C42(H42), C43(H43)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C29(H29A,H29B,
 H29C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              26628
_shelx_fab_checksum              90597
_olex2_submission_special_instructions 'No special instructions were received'