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_4322652
_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            'C45 H60 B Cl Fe O1.25 P4'
_chemical_formula_weight         846.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             1996-07-31
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 107.89(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.938(3)
_cell_length_b                   29.647(4)
_cell_length_c                   13.131(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      10.2
_cell_volume                     4793.2(18)
_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      0.06406
_diffrn_orient_matrix_UB_12      0.01983
_diffrn_orient_matrix_UB_13      0.00567
_diffrn_orient_matrix_UB_21      0.04808
_diffrn_orient_matrix_UB_22      -0.02716
_diffrn_orient_matrix_UB_23      0.01187
_diffrn_orient_matrix_UB_31      -0.01347
_diffrn_orient_matrix_UB_32      -0.00266
_diffrn_orient_matrix_UB_33      -0.07894
_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  0.07146
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6520
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         55.07
_diffrn_reflns_theta_min         3.54
_diffrn_standards_decay_%        0.54
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             1792.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.856
_refine_ls_goodness_of_fit_obs   2.856
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     482
_refine_ls_number_reflns         2129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_obs          0.0915
_refine_ls_shift/esd_max         0.0060
_refine_ls_shift/esd_mean        0.0020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0866
_refine_ls_wR_factor_obs         0.0866
_reflns_number_observed          2129
_reflns_number_total             6198
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic9701928_2.cif
_cod_data_source_block           C45H60BClFeO1.25P4
_cod_depositor_comments
;
 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

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) +
0.00002|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) + 0.00002|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4793(1)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C45 H60 B Cl Fe O1.25 P4 '
_cod_database_code               4322652