Coordination Chemistry of H2 and N2 in Aqueous Solution. Reactivity and Mechanistic Studies Using trans-FeII(P2)2X2-Type Complexes (P2= a Chelating, Water-Solubilizing Phosphine)
John D. Gilbertson; Nathaniel K. Szymczak; Justin L. Crossland; Warren K. Miller; David K. Lyon; Bruce M. Foxman; Joclyn Davis; David R. Tyler; Inorganic Chemistry 46 (2007) 1205–1214; doi:10.1021/ic061570o

data_4307069
_publ_section_title
;
Coordination Chemistry of H2 and N2 in Aqueous Solution. Reactivity and
Mechanistic Studies Using trans-FeII(P2)2X2-Type Complexes (P2= a Chelating,
Water-Solubilizing Phosphine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1205
_journal_page_last               1214
_journal_paper_doi               10.1021/ic061570o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C54.00 H119.50 Cl2 Fe1 O20 P6'
_chemical_formula_sum            'C54 H119.5 Cl2 Fe O20 P6'
_chemical_formula_weight         1401.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-02-16
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 106.718(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5544(19)
_cell_length_b                   14.0778(10)
_cell_length_c                   41.888(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     14432.3(18)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            26802
_diffrn_reflns_theta_full        25.191
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         1.669
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       prism
_exptl_crystal_F_000             6027.966
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         8436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.019923
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +33.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1516
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1280
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              49
_reflns_limit_l_min              0
_reflns_number_gt                8436
_reflns_number_total             14383
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.73
_oxford_diffrn_Wilson_scale      169.99
_oxford_refine_ls_scale          0.08532(2)
_oxford_structure_analysis_title 'jdg16sx in C2/c'
_cod_data_source_file            ic061570osi20060818_015222.cif
_cod_data_source_block           jdg16sx
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        14432.2(18)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C54.00 H119.50 Cl2 Fe1 O20 P6'
_cod_database_code               4307069