Poly[[μ-aqua-aqua[μ~4~-ethyl (dichloromethylene)diphosphonato]sesquicalcium(II)] acetone hemisolvate 4.5-hydrate]
Jokiniemi, Jonna; Peräniemi, Sirpa; Vepsäläinen, Jouko; Ahlgrén, Markku; Acta Crystallographica Section E 65 (2009) m436–m437; doi:10.1107/S1600536809010150

data_2221554
_publ_section_title
;
 Poly[[\m-aqua-aqua[\m~4~-ethyl
 (dichloromethylene)diphosphonato]sesquicalcium(II)] acetone
 hemisolvate 4.5-hydrate]
;
_journal_coeditor_code           XU2487
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m436
_journal_page_last               m437
_journal_paper_doi               10.1107/S1600536809010150
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Ca3 (C3 H5 Cl2 O6 P2)2 (H2 O)2]2, C3 H6 O, 9H2 O'
_chemical_formula_moiety
'C6 H18 Ca3 Cl4 O16 P4, C3 H6 O, 9(H2 O)'
_chemical_formula_sum            'C9 H42 Ca3 Cl4 O26 P4'
_chemical_formula_weight         952.34
_chemical_name_systematic
;
Poly[[\m-aqua-aqua[\m~4~-ethyl
(dichloromethylene)diphosphonato]sesquicalcium(II)] acetone hemisolvate
4.5-hydrate]
;
_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                 103.1070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.2205(3)
_cell_length_b                   10.15460(10)
_cell_length_c                   11.65100(10)
_cell_measurement_reflns_used    31118
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.68
_cell_volume                     3597.51(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31118
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.68
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.9048
_exptl_absorpt_correction_T_min  0.8233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.584
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0303
_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^)+(0.02P)^2^+12P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                3617
_reflns_number_total             4209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2487.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         476.17
_cod_original_formula_moiety
'C3 H9 Ca1.50 Cl2 O8 P2, 0.5(C3 H6 O), 4.5(H2 O)'
_cod_original_formula_iupac
'[Ca1.5 (C3 H5 Cl2 O6 P2) (H2 O)2], 0.5C3 H6 O, 4.5H2 O'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C4.50 H21 Ca1.50 Cl2 O13 P2'
_cod_database_code               2221554
_cod_database_fobs_code          2221554