Permanent porosity and role of sulfonate groups in coordination networks constructed from a new polyfunctional phosphonato-sulfonate linker molecule.
Wöhlbrandt, Stephan; Igeska, Angela; Svensson Grape, Erik; Øien-Ødegaard, Sigurd; Ken Inge, A.; Stock, Norbert; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2724–2733; doi:10.1039/c9dt04571f

data_7703482
_publ_section_title
;
 Permanent porosity and role of sulfonate groups in coordination networks
 constructed from a new polyfunctional phosphonato-sulfonate linker
 molecule.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2724
_journal_page_last               2733
_journal_paper_doi               10.1039/c9dt04571f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C9 H11 N O9 P2 Pb2 S, 0.5(H2 O)'
_chemical_formula_sum            'C9 H12 N O9.5 P2 Pb2 S'
_chemical_formula_weight         794.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.34340(10)
_cell_length_b                   23.6346(3)
_cell_length_c                   13.1707(2)
_cell_measurement_reflns_used    1488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.894
_cell_measurement_theta_min      1.817
_cell_volume                     1662.46(5)
_computing_cell_refinement       'DIALS (Evans, 2018)'
_computing_data_collection       'MXCube3 (Mueller, 2011)'
_computing_data_reduction
;
DIALS (Evans, 2018)
SADABS (Bruker, 2018)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov, 2009)
Diamond (Brandenburg, 2014)
;
_computing_publication_material
;
Encifer (Allen, 2004)
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
Olex2 (Dolomanov, 2009)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
Platon (Spek, 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device       'Biomax (Thunnissen, 2013)'
_diffrn_measurement_device_type  'Eiger 16M detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.1585
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9995
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        22.305
_diffrn_reflns_theta_max         22.305
_diffrn_reflns_theta_min         1.817
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.036
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.5874.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.175
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.5874
_refine_diff_density_max         4.370
_refine_diff_density_min         -3.240
_refine_diff_density_rms         0.712
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.482
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.438
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.1481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3646
_refine_ls_wR_factor_ref         0.3900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1206
_reflns_number_total             1804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04571f2.cif
_cod_data_source_block           PbSPP712B
_cod_depositor_comments
'Adding full bibliography for 7703479--7703482.cif.'
_cod_original_formula_sum        'C9 H12 N O9.50 P2 Pb2 S'
_cod_database_code               7703482
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.667
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H10B-O4
 1.98 with sigma of 0.0002
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.06
4. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C9, C8, C1, C3, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5)
6.a Free rotating group:
 O10(H10A,H10B)
6.b Ternary CH refined with riding coordinates:
 N1(H1)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
6.e Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9)
;
_shelx_res_checksum              1715
_olex2_submission_special_instructions 'No special instructions were received'