Precursors to Water-Soluble Dinitrogen Carriers. Synthesis of Water-Soluble Complexes of Iron(II) Containing Water-Soluble Chelating Phosphine Ligands of the Type 1,2-Bis(bis(hydroxyalkyl)phosphino)ethane
Warren K. Miller; John D. Gilbertson; Carmen Leiva-Paredes; Paul R. Bernatis; Timothy J. R. Weakley; David K. Lyon; David R. Tyler; Inorganic Chemistry 41 (2002) 5453–5465; doi:10.1021/ic025774q

data_4318720
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Precursors to Water-Soluble Dinitrogen Carriers. Synthesis of
 Water-Soluble Complexes of Iron(II) Containing Water-Soluble Chelating
 Phosphine Ligands of the Type 1,2-Bis(bis(hydroxyalkyl)phosphino)ethane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5453
_journal_page_last               5465
_journal_paper_doi               10.1021/ic025774q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C28 H64 Fe O8 P4 2+, O4 S 2-, 0.5(H2 O)'
_chemical_formula_sum            'C28 H65 Fe O12.5 P4 S'
_chemical_formula_weight         813.62
_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'
_cell_angle_alpha                90
_cell_angle_beta                 100.07(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.023(2)
_cell_length_b                   22.427(2)
_cell_length_c                   17.195(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    273
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      13.0
_cell_volume                     3805.6(11)
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      0.01675
_diffrn_orient_matrix_UB_12      0.03347
_diffrn_orient_matrix_UB_13      0.03877
_diffrn_orient_matrix_UB_21      0.08567
_diffrn_orient_matrix_UB_22      -0.01951
_diffrn_orient_matrix_UB_23      0.02611
_diffrn_orient_matrix_UB_31      0.05093
_diffrn_orient_matrix_UB_32      0.02179
_diffrn_orient_matrix_UB_33      -0.03619
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7314
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.22
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Walker & Stuart, 1983'
_exptl_crystal_colour            red-pink
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1740.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.12
_refine_diff_density_min         -1.33
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.99
_refine_ls_goodness_of_fit_ref   2.38
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.126
_refine_ls_R_factor_gt           0.084
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I) + (0.020I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.151
_refine_ls_wR_factor_ref         0.075
_reflns_number_observed          4361
_reflns_number_total             6698
_reflns_observed_criterion       I>1.00\s(I)
_cod_data_source_file            ic025774q_s1_4.cif
_cod_data_source_block           2_C28H64FeO12P4S,0.5H2O
_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 
;
_cod_original_cell_volume        3805(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C28 H65 Fe O12.5 P4 S '
_cod_database_code               4318720