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_4318721
_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_structural     'Fe (C14 H32 O4 P2 )2 (C O ) (O4 S )'
_chemical_formula_sum            'C29 H64 Fe O13 P4 S'
_chemical_formula_weight         832.62
_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                 100.152(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6314(8)
_cell_length_b                   15.943(2)
_cell_length_c                   21.422(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      12.0
_cell_volume                     3910.3(8)
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      -0.03158
_diffrn_orient_matrix_UB_12      -0.00806
_diffrn_orient_matrix_UB_13      0.04007
_diffrn_orient_matrix_UB_21      0.08072
_diffrn_orient_matrix_UB_22      0.00521
_diffrn_orient_matrix_UB_23      0.02511
_diffrn_orient_matrix_UB_31      -0.01089
_diffrn_orient_matrix_UB_32      0.06200
_diffrn_orient_matrix_UB_33      0.00310
_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  0.053
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6250
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        18.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.99
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.02
_refine_ls_goodness_of_fit_ref   2.48
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.130
_refine_ls_R_factor_gt           0.093
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.0018
_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         0.155
_refine_ls_wR_factor_ref         0.078
_reflns_number_observed          3368
_reflns_number_total             5691
_reflns_observed_criterion       I>1.00\s(I)
_cod_data_source_file            ic025774q_s1_5.cif
_cod_data_source_block           9_C29H64FeO13P4S
_cod_original_cell_volume        3910(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C29 H64 Fe O13 P4 S '
_cod_database_code               4318721