A structural study of alkaline earth metal complexes of (dichloromethylene)bisphosphonic acid P-morpholinium- and P-pyrrolidinium-P′-methyl esters
Jokiniemi, Jonna; Peräniemi, Sirpa; Vepsäläinen, Jouko J.; Ahlgrén, Markku; CrystEngComm 10 (2008) 1011–; doi:10.1039/b802668h

data_7202024
_publ_section_title
;
 A structural study of alkaline earth metal complexes of
 (dichloromethylene)bisphosphonic acid P-morpholinium- and
 P-pyrrolidinium-P&#x2032;-methyl esters
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1011
_journal_paper_doi               10.1039/b802668h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C6 H17 Cl2 Mg N O9 P2'
_chemical_formula_sum            'C6 H17 Cl2 Mg N O9 P2'
_chemical_formula_weight         404.36
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.970(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.2714(6)
_cell_length_b                   7.4956(1)
_cell_length_c                   17.4303(4)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.77
_cell_volume                     3059.08(11)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect(Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.0 (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       multi-scan
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20095
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_correction_T_min  0.8703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker AXS, 1998)'
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00136(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0250P)^2^+5.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                3136
_reflns_number_total             3487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802668h.txt
_cod_data_source_block           Structure(1)
_cod_database_code               7202024