Fluorine NMR reporter for phosphate anions
Haiying Gan; Allen G. Oliver; Bradley D. Smith; Chem.Commun. 49 (2013) 5070–; doi:10.1039/c3cc42169d

data_7109339
_publ_section_title
;
 Fluorine NMR reporter for phosphate anions
;
_journal_name_full               Chem.Commun.
_journal_page_first              5070
_journal_paper_doi               10.1039/c3cc42169d
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H34 F N6 O6 P Zn2, 2(N O3), 2.62(H2 O)'
_chemical_formula_sum            'C32 H39.25 F N8 O14.62 P Zn2'
_chemical_formula_weight         950.67
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 108.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2555(19)
_cell_length_b                   19.4335(19)
_cell_length_c                   20.627(2)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.27
_cell_volume                     7704.5(13)
_computing_cell_refinement       'Bruker SAINT v8.18C'
_computing_data_collection       'Bruker APEX-II v2012-6.0'
_computing_data_reduction        'Bruker SAINT v8.18C'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT-2012/1 (Sheldrick, 2012)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            211824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         1.228
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.9197
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             3906
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.471(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2113
_refine_ls_number_reflns         38661
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+4.2733P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                35250
_reflns_number_total             38661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc42169d.txt
_cod_data_source_block           nd1241
_cod_original_cell_volume        7704.7(13)
_cod_database_code               7109339
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.853
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelxl_version_number           2012-6