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_7703481
_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 H23 Mg2 N O15 P2 S, 2(H2 O)'
_chemical_formula_sum            'C9 H27 Mg2 N O17 P2 S'
_chemical_formula_weight         563.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-23
_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                 113.1800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8531(8)
_cell_length_b                   5.3729(2)
_cell_length_c                   23.7906(10)
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.35
_cell_volume                     2215.34(16)
_computing_cell_refinement       'Bruker AXS APEX 3 v2017.3-0'
_computing_data_collection       'Bruker AXS APEX 3 v2017.3-0'
_computing_data_reduction        'Bruker AXS APEX 3 v2017.3-0'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294.32
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.423
_diffrn_reflns_theta_min         2.350
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       rod
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+6.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3763
_reflns_number_total             5014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04571f2.cif
_cod_data_source_block           mg_cau
_cod_depositor_comments
'Adding full bibliography for 7703479--7703482.cif.'
_cod_database_code               7703481
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1B} of O1, {H2A,H2B} of O2, {H5A,H5B} of O5, {H6A,
  H6B} of O6, {H3A,H3B} of O3, {H4A,H4B} of O4, All C(H,H) groups, All N(H)
  groups
 At 1.5 times of:
  {H8C,H8D} of O8, {H7C,H7D} of O7
2. Restrained distances
 H1-N1
 0.95 with sigma of 0.02
 H6A-O6 = H4A-O4 = H5A-O5 = H5B-O5 = H2A-O2 = H2B-O2 = H4B-O4
 0.9 with sigma of 0.02
 O6-H6B = O1-H1B
 0.9 with sigma of 0.02
 Mg2-H5B = Mg2-H5A = Mg1-H1A = Mg1-H1B
 2.6 with sigma of 0.02
 H5B-O8_$1
 2.1 with sigma of 0.02
 H7D-H1B = H7C-H8D = H5B-H8C_$1
 2.1 with sigma of 0.02
 H8C-H5B_$3 = H8D-H5A_$2 = H7C-H8C
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Free rotating group:
 O7(H7C,H7D), O8(H8C,H8D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_shelx_res_checksum              70804
_olex2_submission_special_instructions 'No special instructions were received'