#------------------------------------------------------------------------------
#$Date: 2019-11-05 13:43:04 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223337 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701692.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7701692
loop_
_publ_author_name
'Whitmire, Kenton H.'
'Schipper, Desmond E.'
_publ_section_title
;
 In pursuit of advanced materials from single-source precursors based on
 metal carbonyls.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2248
_journal_page_last               2262
_journal_paper_doi               10.1039/c8dt03406k
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H42 Fe2 O4 P4'
_chemical_formula_sum            'C20 H42 Fe2 O4 P4'
_chemical_formula_weight         582.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'A 2y'
_space_group_name_H-M_alt        'A 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-11-28 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 144.35(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.553(3)
_cell_length_b                   6.68483(14)
_cell_length_c                   22.247(2)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      1.0
_cell_volume                     2908.3(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku, 2015)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.867
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.812
_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            Orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.878
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.432(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         9616
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0354
_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/[σ²(Fo²)+(0.0366P)²+1.1691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                8402
_reflns_number_total             9616
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03406k1.cif
_cod_data_source_block           B
_cod_original_cell_volume        2908.3(10)
_cod_original_sg_symbol_H-M      'a 1 2 1'
_cod_database_code               7701692
_publcif_datablock.id            {9086793c-12e5-456d-9879-5d89bdfd0adc}
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.900
_oxdiff_exptl_absorpt_empirical_full_max 1.101
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x, y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.45694(2) 0.23371(5) 0.49342(3) 0.02062(8) Uani 1 1 d . .
Fe2 Fe 0.02763(2) 0.37964(6) 0.08935(3) 0.02412(9) Uani 1 1 d D .
P1 P 0.44566(3) 0.06261(11) 0.39419(5) 0.02149(13) Uani 1 1 d . .
P2 P 0.39453(4) 0.03467(12) 0.47221(6) 0.02923(16) Uani 1 1 d . .
P3 P 0.06431(3) 0.54651(11) 0.05405(5) 0.02403(14) Uani 1 1 d . .
P4 P 0.05515(5) 0.59121(14) 0.19389(7) 0.0411(2) Uani 1 1 d D .
O12 O 0.50391(14) 0.5325(4) 0.63709(19) 0.0521(7) Uani 1 1 d . .
O21 O 0.13861(15) 0.0880(5) 0.2302(2) 0.0629(8) Uani 1 1 d . .
C101 C 0.36858(14) 0.0589(5) 0.24913(19) 0.0286(6) Uani 1 1 d . .
O11 O 0.35517(13) 0.5331(4) 0.3363(2) 0.0529(7) Uani 1 1 d . .
C301 C 0.15134(14) 0.5478(5) 0.1251(2) 0.0328(6) Uani 1 1 d . .
C12 C 0.48811(15) 0.4100(5) 0.5843(2) 0.0308(6) Uani 1 1 d . .
C203 C 0.44068(19) 0.0730(8) 0.6456(3) 0.0511(10) Uani 1 1 d . .
H20A H 0.460421 -0.058017 0.666479 0.077 Uiso 1 1 calc R U
H20B H 0.430957 0.101274 0.675132 0.077 Uiso 1 1 calc R U
H20C H 0.472266 0.170497 0.669064 0.077 Uiso 1 1 calc R U
C401 C 0.11885(18) 0.5472(7) 0.3315(2) 0.0431(8) Uani 1 1 d D .
C201 C 0.37437(16) 0.0814(6) 0.5279(2) 0.0343(7) Uani 1 1 d . .
O22 O -0.04867(16) 0.0900(5) 0.0671(3) 0.0644(9) Uani 1 1 d . .
C11 C 0.39446(15) 0.4113(5) 0.3959(2) 0.0302(6) Uani 1 1 d . .
C403 C 0.1235(2) 0.7279(9) 0.3787(3) 0.0656(12) Uani 1 1 d . .
H40A H 0.140390 0.840821 0.377313 0.098 Uiso 1 1 calc R U
H40B H 0.153997 0.698495 0.448703 0.098 Uiso 1 1 calc R U
H40C H 0.078900 0.758084 0.339715 0.098 Uiso 1 1 calc R U
C21 C 0.09609(17) 0.2077(5) 0.1738(3) 0.0380(7) Uani 1 1 d . .
C22 C -0.02049(17) 0.2073(5) 0.0731(3) 0.0367(7) Uani 1 1 d . .
C303 C 0.1835(2) 0.3413(7) 0.1626(4) 0.0651(14) Uani 1 1 d . .
H30A H 0.194730 0.299388 0.216393 0.098 Uiso 1 1 calc R U
H30B H 0.224395 0.345737 0.188783 0.098 Uiso 1 1 calc R U
H30C H 0.151855 0.248243 0.106323 0.098 Uiso 1 1 calc R U
C304 C 0.1446(2) 0.6228(8) 0.0526(4) 0.0616(12) Uani 1 1 d . .
H30D H 0.116710 0.531625 -0.004189 0.092 Uiso 1 1 calc R U
H30E H 0.189078 0.631327 0.089119 0.092 Uiso 1 1 calc R U
H30F H 0.123649 0.752663 0.027053 0.092 Uiso 1 1 calc R U
C102 C 0.3803(2) -0.1026(10) 0.2165(3) 0.0722(16) Uani 1 1 d . .
H10A H 0.419528 -0.068735 0.240697 0.108 Uiso 1 1 calc R U
H10B H 0.340800 -0.112627 0.142652 0.108 Uiso 1 1 calc R U
H10C H 0.388008 -0.228498 0.245579 0.108 Uiso 1 1 calc R U
C204 C 0.3247(2) -0.0800(9) 0.4893(4) 0.0642(13) Uani 1 1 d . .
H20D H 0.282631 -0.071153 0.415639 0.096 Uiso 1 1 calc R U
H20E H 0.315641 -0.060141 0.520224 0.096 Uiso 1 1 calc R U
H20F H 0.344613 -0.209747 0.507812 0.096 Uiso 1 1 calc R U
C302 C 0.19617(19) 0.6883(9) 0.2165(3) 0.0716(16) Uani 1 1 d . .
H30G H 0.178526 0.821982 0.192006 0.107 Uiso 1 1 calc R U
H30H H 0.241986 0.685011 0.257135 0.107 Uiso 1 1 calc R U
H30I H 0.196338 0.646729 0.257963 0.107 Uiso 1 1 calc R U
C104 C 0.30688(16) -0.0009(6) 0.2112(2) 0.0449(9) Uani 1 1 d . .
H10D H 0.314929 -0.129457 0.238948 0.067 Uiso 1 1 calc R U
H10E H 0.267071 -0.007485 0.137253 0.067 Uiso 1 1 calc R U
H10F H 0.299753 0.096591 0.233541 0.067 Uiso 1 1 calc R U
C202 C 0.3418(2) 0.2888(7) 0.4929(4) 0.0586(12) Uani 1 1 d . .
H20G H 0.373339 0.387697 0.516987 0.088 Uiso 1 1 calc R U
H20H H 0.330929 0.316257 0.520823 0.088 Uiso 1 1 calc R U
H20I H 0.300785 0.292665 0.418971 0.088 Uiso 1 1 calc R U
C103 C 0.3554(2) 0.2570(7) 0.2033(3) 0.0638(13) Uani 1 1 d . .
H10G H 0.350947 0.358839 0.228069 0.096 Uiso 1 1 calc R U
H10H H 0.313875 0.249580 0.129476 0.096 Uiso 1 1 calc R U
H10I H 0.392794 0.289361 0.222993 0.096 Uiso 1 1 calc R U
C404 C 0.0997(4) 0.3625(11) 0.3422(5) 0.112(3) Uani 1 1 d . .
H40D H 0.055072 0.379265 0.304695 0.169 Uiso 1 1 calc R U
H40E H 0.132420 0.340060 0.413776 0.169 Uiso 1 1 calc R U
H40F H 0.099453 0.249830 0.315143 0.169 Uiso 1 1 calc R U
C402 C 0.1884(2) 0.5233(13) 0.3862(3) 0.101(2) Uani 1 1 d . .
H40G H 0.189633 0.398763 0.366199 0.152 Uiso 1 1 calc R U
H40H H 0.223849 0.524410 0.459470 0.152 Uiso 1 1 calc R U
H40I H 0.195488 0.631754 0.367234 0.152 Uiso 1 1 calc R U
H1 H 0.4525(16) -0.136(6) 0.409(2) 0.031(9) Uiso 1 1 d . .
H3 H 0.0544(18) 0.743(6) 0.041(3) 0.041(10) Uiso 1 1 d . .
H2A H 0.4125(19) -0.147(6) 0.497(3) 0.043(10) Uiso 1 1 d . .
H4A H 0.071(3) 0.776(9) 0.198(4) 0.10(2) Uiso 1 1 d D .
H2B H 0.333(2) 0.014(7) 0.378(3) 0.059(13) Uiso 1 1 d . .
H4B H 0.000(3) 0.649(9) 0.167(4) 0.10(2) Uiso 1 1 d D .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C11 Fe1 C12 87.99(15) . .
C11 Fe1 P2 99.86(11) . .
C12 Fe1 P2 103.02(11) . .
C11 Fe1 P1 156.71(10) . 2_656
C12 Fe1 P1 95.37(11) . 2_656
P2 Fe1 P1 101.79(4) . 2_656
C11 Fe1 P1 92.98(10) . .
C12 Fe1 P1 160.06(11) . .
P2 Fe1 P1 96.43(3) . .
P1 Fe1 P1 76.21(4) 2_656 .
C11 Fe1 Fe1 103.58(10) . 2_656
C12 Fe1 Fe1 107.07(10) . 2_656
P2 Fe1 Fe1 142.14(2) . 2_656
P1 Fe1 Fe1 53.41(2) 2_656 2_656
P1 Fe1 Fe1 53.37(3) . 2_656
C21 Fe2 C22 88.59(16) . .
C21 Fe2 P4 103.28(12) . .
C22 Fe2 P4 99.55(12) . .
C21 Fe2 P3 160.47(12) . 2
C22 Fe2 P3 93.55(11) . 2
P4 Fe2 P3 95.52(4) . 2
C21 Fe2 P3 95.04(12) . .
C22 Fe2 P3 158.65(11) . .
P4 Fe2 P3 100.06(4) . .
P3 Fe2 P3 76.25(4) 2 .
C21 Fe2 Fe2 108.11(12) . 2
C22 Fe2 Fe2 106.22(11) . 2
P4 Fe2 Fe2 139.42(3) . 2
P3 Fe2 Fe2 52.71(3) 2 2
P3 Fe2 Fe2 52.69(3) . 2
C101 P1 Fe1 130.55(11) . 2_656
C101 P1 Fe1 126.59(10) . .
Fe1 P1 Fe1 73.22(3) 2_656 .
C201 P2 Fe1 123.93(12) . .
C301 P3 Fe2 127.27(11) . 2
C301 P3 Fe2 129.30(11) . .
Fe2 P3 Fe2 74.60(3) 2 .
C401 P4 Fe2 125.57(14) . .
C103 C101 C102 110.5(4) . .
C103 C101 C104 109.7(3) . .
C102 C101 C104 108.2(3) . .
C103 C101 P1 112.9(2) . .
C102 C101 P1 107.4(2) . .
C104 C101 P1 108.0(2) . .
C303 C301 C302 109.8(4) . .
C303 C301 C304 108.0(4) . .
C302 C301 C304 110.3(4) . .
C303 C301 P3 112.6(2) . .
C302 C301 P3 107.5(2) . .
C304 C301 P3 108.6(2) . .
O12 C12 Fe1 174.8(3) . .
C404 C401 C403 111.1(4) . .
C404 C401 C402 111.2(5) . .
C403 C401 C402 107.4(4) . .
C404 C401 P4 109.2(3) . .
C403 C401 P4 110.5(3) . .
C402 C401 P4 107.4(3) . .
C202 C201 C203 110.4(4) . .
C202 C201 C204 110.5(3) . .
C203 C201 C204 109.9(3) . .
C202 C201 P2 108.0(2) . .
C203 C201 P2 108.9(2) . .
C204 C201 P2 109.1(3) . .
O11 C11 Fe1 176.6(3) . .
O21 C21 Fe2 174.6(3) . .
O22 C22 Fe2 176.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C11 1.766(3) .
Fe1 C12 1.770(3) .
Fe1 P2 2.1845(9) .
Fe1 P1 2.2273(11) 2_656
Fe1 P1 2.2285(8) .
Fe1 Fe1 2.6571(8) 2_656
Fe2 C21 1.765(3) .
Fe2 C22 1.765(3) .
Fe2 P4 2.1844(10) .
Fe2 P3 2.2235(13) 2
Fe2 P3 2.2242(8) .
Fe2 Fe2 2.6953(10) 2
P1 C101 1.881(3) .
P2 C201 1.859(3) .
P3 C301 1.877(3) .
P4 C401 1.841(3) .
O12 C12 1.149(4) .
O21 C21 1.158(4) .
C101 C103 1.502(5) .
C101 C102 1.521(5) .
C101 C104 1.523(4) .
O11 C11 1.148(4) .
C301 C303 1.518(5) .
C301 C302 1.519(5) .
C301 C304 1.520(5) .
C203 C201 1.530(5) .
C401 C404 1.498(8) .
C401 C403 1.523(6) .
C401 C402 1.530(6) .
C201 C202 1.530(6) .
C201 C204 1.534(6) .
O22 C22 1.149(4) .
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
