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_4318719
_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         'C37 H80 Cl Fe O9 P4 1+, C24 H20 B 1-'
_chemical_formula_sum            'C61 H100 B Cl Fe O9 P4'
_chemical_formula_weight         1203.46
_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                91.61(3)
_cell_angle_beta                 99.18(2)
_cell_angle_gamma                100.93(3)
_cell_formula_units_Z            2
_cell_length_a                   10.495(2)
_cell_length_b                   13.037(4)
_cell_length_c                   24.809(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.0
_cell_volume                     3284.2(15)
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.09020
_diffrn_orient_matrix_UB_12      0.01650
_diffrn_orient_matrix_UB_13      -0.00441
_diffrn_orient_matrix_UB_21      0.02005
_diffrn_orient_matrix_UB_22      0.03292
_diffrn_orient_matrix_UB_23      0.03809
_diffrn_orient_matrix_UB_31      0.03385
_diffrn_orient_matrix_UB_32      0.06904
_diffrn_orient_matrix_UB_33      -0.01431
_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  0.021
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9107
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        8.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1292.00
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.53
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.78
_refine_ls_goodness_of_fit_ref   1.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.088
_refine_ls_R_factor_gt           0.063
_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         0.114
_refine_ls_wR_factor_ref         0.057
_reflns_number_observed          6254
_reflns_number_total             8558
_reflns_observed_criterion       I>1.00\s(I)
_cod_data_source_file            ic025774q_s1_3.cif
_cod_data_source_block           8_C61H100BClFeO9P4
_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        3284(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C61 H100 B Cl Fe O9 P4 '
_cod_database_code               4318719