A heterofunctional ligand approach for the preparation of high connectivity coordination polymers: combining a “bridge” and “pillar” in one ligand
AL-Fayaad, Hydar; Arachchige, Kasun; Clegg, Jack Kay; CrystEngComm  (2020) –; doi:10.1039/D0CE01020K

data_7240905
_publ_section_title
;
 A heterofunctional ligand approach for the preparation of high
 connectivity coordination polymers: combining a &#x201C;bridge&#x201D;
 and &#x201C;pillar&#x201D; in one ligand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01020K
_journal_year                    2020
_chemical_formula_moiety
'H20 Na2 O10, C18 H12 N2 O4, C18 H10 N2 O4, 8(H2 O)'
_chemical_formula_sum            'C36 H58 N4 Na2 O26'
_chemical_formula_weight         1008.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-10 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                101.580(7)
_cell_angle_beta                 98.222(6)
_cell_angle_gamma                117.146(6)
_cell_formula_units_Z            1
_cell_length_a                   10.4109(6)
_cell_length_b                   11.1279(7)
_cell_length_c                   12.1125(10)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.123
_cell_measurement_theta_min      3.566
_cell_volume                     1178.13(17)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4205
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         3.566
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   25.123
_exptl_transmission_factor_min   3.566
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4205
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.267
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+3.8075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3706
_reflns_number_total             4205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01020k1.cif
_cod_data_source_block           Na2(H2L)L
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1178.13(15)
_cod_database_code               7240905
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.855(4)
 0.145(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All H(H) groups, All H(H,H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 H2N-N2N
 0.84 with sigma of 0.02
 O5-H5B
 0.88 with sigma of 0.02
 O5-H5A
 0.88 with sigma of 0.02
 H10B-O10
 0.87 with sigma of 0.02
 H11B-O11
 0.87 with sigma of 0.02
 H9B-O9
 0.87 with sigma of 0.02
 O6-H6B
 0.87 with sigma of 0.02
 O13-H13A
 0.87 with sigma of 0.02
 O13-H13B
 0.87 with sigma of 0.02
4.a Free rotating group:
 O11(H11A), O10(H10A), O12(H12A,H12B)
4.b Rotating group:
 O9(H9A), O8(H8A,H8B), O6(H6A), O7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              34049
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'