Iron(II) Complexes Containing the 1,2-Diphospholanoethane Ligand
Leslie D. Field; Iain P. Thomas; Trevor W. Hambley; Peter Turner; Inorganic Chemistry 37 (1998) 612–618; doi:10.1021/ic9701928

data_4322651
_publ_contact_author
;
    Prof. Leslie D. Field
 School of Chemistry, University of Sydney, Sydney, NSW 2006, Australia
;
_publ_contact_author_email       ' l.field@chem.usyd.edu.au '
_publ_contact_author_fax         ' 61-2-9351 3329 '
_publ_section_title
;
 Iron(II) Complexes Containing the 1,2-Diphospholanoethane Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              612
_journal_page_last               618
_journal_paper_doi               10.1021/ic9701928
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C24 H48 Cl2 Fe O P4'
_chemical_formula_weight         603.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             1997-08-26
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 101.77(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.084(3)
_cell_length_b                   14.059(2)
_cell_length_c                   17.665(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      9.7
_cell_volume                     2938.0(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.02446
_diffrn_orient_matrix_UB_12      -0.06068
_diffrn_orient_matrix_UB_13      0.02799
_diffrn_orient_matrix_UB_21      0.06698
_diffrn_orient_matrix_UB_22      -0.00292
_diffrn_orient_matrix_UB_23      -0.02511
_diffrn_orient_matrix_UB_31      0.04539
_diffrn_orient_matrix_UB_32      0.03700
_diffrn_orient_matrix_UB_33      0.04393
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.03792
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5117
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         50.04
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        -10.12
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.966
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.25
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_refine_diff_density_max         0.90
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       0.000002444
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_obs   2.960
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     290
_refine_ls_number_reflns         2489
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0720
_refine_ls_shift/esd_max         0.0100
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0680
_reflns_number_observed          2489
_reflns_number_total             4819
_reflns_observed_criterion       >2.50\s(I)
_cod_data_source_file            ic9701928_1.cif
_cod_data_source_block           C24H48Cl2FeOP4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2938.0(8)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C24 H48 Cl2 Fe O P4 '
_cod_database_code               4322651