Two fluorescent lead phosphonates for highly selective sensing of nitro aromatics (NACs), Fe3+ and MnO4− ions
Xing, Bo; Li, Huan-Yu; Zhu, Yanyu; Zhao, Zhou; Sun, Zhen-Gang; Yang, Dan; Li, Jing; RSC Adv.  (2016) –; doi:10.1039/C6RA21403G

data_7227000
_publ_section_title
;
 Two fluorescent lead phosphonates for highly selective sensing of nitro
 aromatics (NACs), Fe3+ and MnO4&#x2212; ions
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA21403G
_journal_year                    2016
_chemical_formula_moiety         'C51 H48 O21 P3 Pb3'
_chemical_formula_sum            'C51 H47 O21 P3 Pb3'
_chemical_formula_weight         1710.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-06
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.09.27 svn.r3342 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-10-27 deposited with the CCDC.
2016-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                96.6760(10)
_cell_angle_beta                 94.1210(10)
_cell_angle_gamma                111.1240(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1420(5)
_cell_length_b                   15.4695(6)
_cell_length_c                   15.6819(6)
_cell_measurement_reflns_used    5083
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      2.27
_cell_volume                     2708.33(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15564
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    9.469
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11054
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.1462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8484
_reflns_number_total             11054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra21403g2.cif
_cod_data_source_block           szg241
_cod_database_code               7227000
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.557
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 P2-O1AA \\sim P2-O0AA
 with sigma of 0.02
 C16A-C0AA \\sim C1AB-C16B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1AB) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2AA) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1AB) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O0AA, C16B, C1AB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P1, O3, C1AA, C2AA
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O1AA, C16B, C1AB
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O0AA, C16A, C0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O2AA(0.6) O0AA(0.6) O3AA(0.4) C16B(0.4) H16A(0.4) H16B(0.4)
 C1AB(0.4) H1AA(0.4) H1AB(0.4) H1AC(0.4) O1AA(0.4) C16A(0.6) H16C(0.6)
 H16D(0.6) C0AA(0.6) H0AA(0.6) H0AB(0.6) H0AC(0.6)
6.a Riding coordinates:
 O13(H13), O15(H15), O21(H21), C1(H1A,H1B), C3(H3), C4(H4), C6(H6), C7(H7),
 C9(H9), C10(H10), C12(H12), C13(H13A), C14(H14A,H14B), C19(H19A,H19B),
 C21(H21A), C22(H22), C24(H24), C25(H25), C26(H26A,H26B), C30(H30), C31(H31),
 C33(H33), C34(H34), C38(H38), C39(H39), C41(H41), C42(H42), C46(H46), C47(H47),
  C49(H49), C50(H50)
6.b Secondary CH2 refined with riding coordinates:
 C16B(H16A,H16B), C1AA(H1AD,H1AE), C16A(H16C,H16D)
6.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C1AB(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C0AA(H0AA,
 H0AB,H0AC)
;
_shelx_res_checksum              78533
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'