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_4307070
_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         'C36 H56 Fe1 O12 P4 S1'
_chemical_formula_sum            'C36 H56 Fe O12 P4 S'
_chemical_formula_weight         892.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-02-21
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 94.83(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.379(3)
_cell_length_b                   15.967(5)
_cell_length_c                   19.943(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    296
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4562.4(19)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7327
_diffrn_reflns_theta_full        23.478
_diffrn_reflns_theta_max         23.478
_diffrn_reflns_theta_min         1.636
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.7782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.031392
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.04 1.34 1.46 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1712
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0876
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3756
_reflns_number_total             6722
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.75
_oxford_diffrn_Wilson_scale      23.86
_oxford_refine_ls_scale          0.2550(9)
_oxford_structure_analysis_title jg1202
_cod_data_source_file            ic061570osi20060818_015241.cif
_cod_data_source_block           CRYSTALS_cif
_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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C36 H56 Fe1 O12 P4 S1'
_cod_database_code               4307070