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_4318723
_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 Br2 Fe O8 P4 '
_chemical_formula_structural     'Fe (C18 H40 O4 P2)2 Br2'
_chemical_formula_sum            'C36 H80 Br2 Fe O8 P4'
_chemical_formula_weight         980.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 111.76(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.750(2)
_cell_length_b                   12.780(3)
_cell_length_c                   20.078(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.0
_cell_volume                     4706.7(18)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.01421
_diffrn_orient_matrix_UB_12      -0.06949
_diffrn_orient_matrix_UB_13      -0.01368
_diffrn_orient_matrix_UB_21      -0.04960
_diffrn_orient_matrix_UB_22      -0.02794
_diffrn_orient_matrix_UB_23      -0.00755
_diffrn_orient_matrix_UB_31      -0.01760
_diffrn_orient_matrix_UB_32      0.02263
_diffrn_orient_matrix_UB_33      -0.05128
_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  0.018
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4472
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0.85
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews, 1968'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2064.00
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.63
_refine_ls_goodness_of_fit_ref   1.76
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.042
_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         0.080
_refine_ls_wR_factor_ref         0.040
_reflns_number_gt                3299
_reflns_number_total             4334
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            ic025774q_s1_7.cif
_cod_data_source_block           5_C36H80Br2FeO8P4
_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        4707(2)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C36 H80 Br2 Fe O8 P4 '
_cod_database_code               4318723