Self assembly of a novel water soluble iron(ii) macrocyclic phosphine complex from tetrakis(hydroxymethyl)phosphonium sulfate and iron(ii) ammonium sulfate: single crystal X-ray structure of the complex [Fe(H2O)2{RP(CH2N(CH2PR2)CH2)2PR}]SO4·4H2O (R = CH2OH)
Jeffery, John C.; Odell, Barbara; Stevens, Nicola; Talbot, Robert E.; Chemical Communications  (2000) 101–; doi:10.1039/a908309j

data_7110767
_publ_section_title
;
 Self assembly of a novel water soluble iron(ii) macrocyclic phosphine
 complex from tetrakis(hydroxymethyl)phosphonium sulfate and iron(ii)
 ammonium sulfate: single crystal X-ray structure of the complex
 [Fe(H2O)2{RP(CH2N(CH2PR2)CH2)2PR}]SO4&#x00B7;4H2O (R = CH2OH)
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              101
_journal_paper_doi               10.1039/a908309j
_journal_year                    2000
_chemical_formula_sum            'C12 H42 Fe N2 O16 P4 S'
_chemical_formula_weight         682.27
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.68(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.106(4)
_cell_length_b                   14.103(6)
_cell_length_c                   15.032(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2566.2(15)
_computing_data_collection       'Siemens/Bruker SMART area detector '
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7820
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.995
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.946
_refine_ls_goodness_of_fit_obs   1.023
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2912
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0809
_refine_ls_wR_factor_obs         0.0756
_reflns_number_observed          2414
_reflns_number_total             2914
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908309jsup1.cif
_cod_data_source_block           od
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2566.3(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7110767