Transformations in Transition-Metal Carbonyls Containing Arsenic: Exploring the Chemistry of [Et4N]2[HAs{Fe(CO)4}3] in the Search for Single-Source Precursors for Advanced Metal Pnictide Materials
Schipper, Desmond E.; Young, Benjamin E.; Whitmire, Kenton H.; Organometallics 35 (2016) 471–; doi:10.1021/acs.organomet.5b00906

data_4088176
_publ_section_title
;
 Transformations in Transition-Metal Carbonyls Containing Arsenic:
 Exploring the Chemistry of [Et4N]2[HAs{Fe(CO)4}3] in the Search for
 Single-Source Precursors for Advanced Metal Pnictide Materials
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              471
_journal_paper_doi               10.1021/acs.organomet.5b00906
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         '(C8 H20 N +) (C15 H As Fe3 Mn O15 -)'
_chemical_formula_sum            'C23 H21 As Fe3 Mn N O15'
_chemical_formula_weight         848.82
_chemical_name_systematic
;
Tetraethylammonium (?2-carbonyl)-(?2-hydrido)-(?4-arsenic)-pentadecacarbonyl-tri-iron-manganese
;
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.531(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.620(8)
_cell_length_b                   14.615(9)
_cell_length_c                   17.279(11)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      1.6
_cell_volume                     3177(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.945
_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_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39798
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.970
_diffrn_reflns_theta_min         1.619
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         10393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+3.0997P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8616
_reflns_number_total             10393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00906_si_002.cif
_cod_data_source_block           VII
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3177(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088176
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.946
_shelxl_version_number           2013-2
_shelx_res_checksum              8567
_shelx_hkl_checksum              64100