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_7011534
_publ_section_title
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 A structural study of bisphosphonate metal complexes. Alkaline earth
 metal complexes of (dichloromethylene)bisphosphonic acid P,P'-diethyl
 ester
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_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         (C5H10NH2)2Cl2C[PO3(C2H5)]2
_chemical_formula_sum            'C15 H34 Cl2 N2 O6 P2'
_chemical_formula_weight         471.28
_space_group_IT_number           2
_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                105.774(1)
_cell_angle_beta                 98.221(2)
_cell_angle_gamma                106.067(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4317(2)
_cell_length_b                   11.2372(3)
_cell_length_c                   11.9292(4)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      3.12
_cell_volume                     1136.17(6)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19610
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_correction_T_min  0.8379
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      1.355(14)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       irregular
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0010(11)
_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   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                4663
_reflns_number_total             5368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201124g.txt
_cod_data_source_block           Structure_1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.7000P] 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^)+(0.0250P)^2^+0.7000P] 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        1136.17(5)
_cod_database_code               7011534