Metal Phosphonates Based on Bis(benzimidazol-2-ylmethyl)imino Methylenephosphonate: From Discrete Dimer to Two-Dimensional Network Containing Metallomacrocycles
Deng-Ke Cao; Jing Xiao; Jian-Wei Tong; Yi-Zhi Li; Li-Min Zheng; Inorganic Chemistry 46 (2007) 428–436; doi:10.1021/ic060990a

data_4306873
_publ_section_title
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Metal Phosphonates Based on Bis(benzimidazol-2-ylmethyl)imino
Methylenephosphonate: From Discrete Dimer to Two-Dimensional Network
Containing Metallomacrocycles
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              428
_journal_page_last               436
_journal_paper_doi               10.1021/ic060990a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C34 H32 Fe2 N10 O6 P2, 0.5(H2 O), 0.5(H2 O)'
_chemical_formula_sum            'C34 H34 Fe2 N10 O7 P2'
_chemical_formula_weight         868.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.330(3)
_cell_angle_beta                 85.224(3)
_cell_angle_gamma                62.268(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5807(14)
_cell_length_b                   9.9959(15)
_cell_length_c                   11.4230(17)
_cell_measurement_reflns_used    802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.79
_cell_measurement_theta_min      2.31
_cell_volume                     962.7(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4760
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         3980
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+1.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3415
_reflns_number_total             3980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060990asi20060604_051747_3.cif
_cod_data_source_block           Fe2{[(C7H5N2)CH2]2NCH2PO3}2.2H2O
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '
_cod_database_code               4306873