Synthesis of 4-Phosphonobutanesulfonic Acid and Systematic Investigation of Copper Phosphonatobutanesulfonates by High-Throughput Methods
Sonnauer, Andreas; Feyand, Mark; Stock, Norbert; Crystal Growth & Design 9 (2009) 586–; doi:10.1021/cg8008865

data_4509112
_publ_section_title
;
 Synthesis of 4-Phosphonobutanesulfonic Acid and Systematic Investigation
 of Copper Phosphonatobutanesulfonates by High-Throughput Methods
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              586
_journal_paper_doi               10.1021/cg8008865
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C4 H12.3 Cu1.50 O8.15 P S'
_chemical_formula_sum            'C4 H12.3 Cu1.5 O8.15 P S'
_chemical_formula_weight         349.09
_chemical_name_systematic
; 
 ? 
;
_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                108.388(11)
_cell_angle_beta                 95.656(11)
_cell_angle_gamma                93.521(11)
_cell_formula_units_Z            2
_cell_length_a                   5.1197(5)
_cell_length_b                   10.5328(10)
_cell_length_c                   10.8003(10)
_cell_measurement_temperature    293(2)
_cell_volume                     547.33(10)
_computing_data_reduction        XPrep
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'STOE IPDS I'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5965
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.6506
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany) 
;
_exptl_crystal_colour            'lightly blue'
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             351
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.011(2)
_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   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                2103
_reflns_number_total             2531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg8008865sup1.cif
_cod_data_source_block           '[Cu1.5(O3P-C4H8-SO3)(H2O)]1.15H2O'
_cod_original_cell_volume        547.3(1)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C4 H12.3 Cu1.50 O8.15 P S'
_cod_database_code               4509112