Building layered structures from hydrogen bonded molecular units and 1D metal phosphonate chains: synthesis, characterization and crystal structures of N,N???-dimethyl-N,N???-ethylenediamine-bis(methylenephosphonic acid), its Ni(ii) and Pb(ii) complexes
Mao, Jiang-Gao; Wang, Zhike; Clearfield, Abraham; Journal of the Chemical Society, Dalton Transactions  (2002) 4541–; doi:10.1039/b206343n

data_7011978
_publ_section_title
;
 Building layered structures from hydrogen bonded molecular units and
 1D metal phosphonate chains: synthesis, characterization and crystal
 structures of
 N,N???-dimethyl-N,N???-ethylenediamine-bis(methylenephosphonic acid),
 its Ni(ii) and Pb(ii) complexes
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4541
_journal_paper_doi               10.1039/b206343n
_journal_year                    2002
_chemical_formula_sum            'C6 H20 N2 Ni O8 P2'
_chemical_formula_weight         368.89
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.577(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.302(7)
_cell_length_b                   9.042(7)
_cell_length_c                   9.932(8)
_cell_measurement_temperature    110(2)
_cell_volume                     688.4(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'Narrow frame method, hemisphere'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4068
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   'psi scan method'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+1.0699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                1328
_reflns_number_total             1571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206343n.txt
_cod_data_source_block           mao15
_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        688.4(9)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7011978