In pursuit of advanced materials from single-source precursors based on metal carbonyls.
Whitmire, Kenton H.; Schipper, Desmond E.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2248–2262; doi:10.1039/c8dt03406k

data_7701692
_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 \w-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/[\s^2^(Fo^2^)+(0.0366P)^2^+1.1691P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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
;
_shelx_res_checksum              13892