A structural study of bisphosphonate metal complexes. Alkaline earth metal complexes of (dichloromethylene)bisphosphonic acid P,P'-diethyl ester
Kontturi, Mervi; Vuokila-Laine, Eija; Peräniemi, Sirpa; Pakkanen, Tuula T.; Vepsäläinen, Jouko J.; Ahlgrén, Markku; Journal of the Chemical Society, Dalton Transactions  (2002) 1969–; doi:10.1039/b201124g

data_7011536
_publ_section_title
;
 A structural study of bisphosphonate metal complexes. Alkaline earth
 metal complexes of (dichloromethylene)bisphosphonic acid P,P'-diethyl
 ester
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1969
_journal_paper_doi               10.1039/b201124g
_journal_year                    2002
_chemical_formula_moiety         '[(H2O)3Ca{Cl2C(PO3Et)2}2Ca(H2O)3]'
_chemical_formula_sum            'C10 H32 Ca2 Cl4 O18 P4'
_chemical_formula_weight         786.20
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0044(4)
_cell_length_b                   15.5269(2)
_cell_length_c                   7.9701(1)
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      3.00
_cell_volume                     2970.57(7)
_computing_cell_refinement       'Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'collect (Nonius, 1999)'
_computing_data_reduction        'Denzo, Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       phi-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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25221
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.8204
_exptl_absorpt_correction_T_min  0.8204
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      1.700(11)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0400P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                1803
_reflns_number_total             2020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201124g.txt
_cod_data_source_block           Structure_3
_cod_original_sg_symbol_H-M      Cmca
_cod_database_code               7011536