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_7028299
_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 H24 Ni O14 P2'
_chemical_formula_sum            'C16 H24 Ni O14 P2'
_chemical_formula_weight         561.00
_chemical_name_systematic
; 
 bis(\m~2~-4-(Phosphatomethyl)benzoic acid)-tetraaqua-nickel
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                83.42(3)
_cell_angle_beta                 89.71(3)
_cell_angle_gamma                83.50(3)
_cell_formula_units_Z            1
_cell_length_a                   4.7713(10)
_cell_length_b                   6.8621(14)
_cell_length_c                   16.598(3)
_cell_measurement_temperature    293(2)
_cell_volume                     536.37(19)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) 
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 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 0.953
_diffrn_measured_fraction_theta_max 0.954
_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    0.0202
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2458
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.7625
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.1682
_exptl_crystal_size_mid          0.1136
_exptl_crystal_size_min          0.0822
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.762
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.762
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0320
_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          0.0427
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                2083
_reflns_number_total             2458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52576g.txt
_cod_data_source_block           c:\einkris\nil6_ipds2\absc\nil6a
_cod_original_cell_volume        536.36(19)
_cod_database_code               7028299