High-throughput ultrasonic synthesis and in situ crystallisation investigation of metal phosphonocarboxylates.
Schilling, Lars-Hendrik; Stock, Norbert; Dalton transactions (Cambridge, England : 2003) 43 (2014) 414–422; doi:10.1039/c3dt52576g

data_7028298
_publ_section_title
;
 High-throughput ultrasonic synthesis and in situ crystallisation
 investigation of metal phosphonocarboxylates.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              414
_journal_page_last               422
_journal_paper_doi               10.1039/c3dt52576g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C16 H20 Ca O12 P2'
_chemical_formula_sum            'C16 H20 Ca O12 P2'
_chemical_formula_weight         506.34
_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                83.84(3)
_cell_angle_beta                 89.03(3)
_cell_angle_gamma                85.65(3)
_cell_formula_units_Z            1
_cell_length_a                   4.6806(9)
_cell_length_b                   6.1340(12)
_cell_length_c                   17.932(4)
_cell_measurement_temperature    293(2)
_cell_volume                     510.37(18)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPSD-2'
_diffrn_measurement_method       'omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2768
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.8853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.1628
_exptl_crystal_size_mid          0.1075
_exptl_crystal_size_min          0.0676
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0411
_reflns_number_gt                1938
_reflns_number_total             2768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52576g.txt
_cod_data_source_block           c:\einkris\lars\absc\lhs1
_cod_original_cell_volume        510.38(17)
_cod_database_code               7028298