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_4318718
_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         'C36 H80 Cl2 Fe O8 P4 '
_chemical_formula_sum            'C36 H80 Cl2 Fe O8 P4'
_chemical_formula_weight         891.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                64.98(4)
_cell_angle_beta                 81.00(2)
_cell_angle_gamma                67.12(4)
_cell_formula_units_Z            1
_cell_length_a                   10.487(3)
_cell_length_b                   10.553(6)
_cell_length_c                   12.432(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      15.0
_cell_volume                     1148.6(9)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05495
_diffrn_orient_matrix_UB_12      -0.04853
_diffrn_orient_matrix_UB_13      -0.05472
_diffrn_orient_matrix_UB_21      -0.08738
_diffrn_orient_matrix_UB_22      0.02579
_diffrn_orient_matrix_UB_23      -0.04035
_diffrn_orient_matrix_UB_31      0.00755
_diffrn_orient_matrix_UB_32      0.09771
_diffrn_orient_matrix_UB_33      -0.05707
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4274
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             480.00
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '2.3(2) \\times 10^-6^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.04
_refine_ls_goodness_of_fit_ref   2.07
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     393
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.0008
_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         0.076
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                3550
_reflns_number_total             4033
_reflns_threshold_expression     I>1.0\s(I)
_cod_data_source_file            ic025774q_s1_2.cif
_cod_data_source_block           1_C36H80Cl2FeO8P4
_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        1149(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H80 Cl2 Fe O8 P4 '
_cod_database_code               4318718