Synthesis, structure and properties of coordination polymers formed from bridging 4-hydroxybenzoic acid anions
Abrahams, Brendan F.; Commons, Christopher J.; Dharma, A. David; Hudson, Timothy A.; Robson, Richard; Sanchez Arlt, Robin W.; Stewart, Thomas C.; White, Keith F.; CrystEngComm  (2022) –; doi:10.1039/D2CE00163B

data_7244470
_publ_section_title
;
 Synthesis, structure and properties of coordination polymers formed from
 bridging 4-hydroxybenzoic acid anions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00163B
_journal_year                    2022
_chemical_formula_moiety         'C14 H14 Mg O8, C4 H8 O2'
_chemical_formula_sum            'C18 H22 Mg O10'
_chemical_formula_weight         422.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.395(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9854(4)
_cell_length_b                   15.4568(5)
_cell_length_c                   12.8852(5)
_cell_measurement_reflns_used    1552
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      73.4010
_cell_measurement_theta_min      5.7100
_cell_volume                     2022.88(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     15.00  57.00   1.00    1.95    --   40.81 -57.00 -90.00   42
  2  \w     34.00  87.00   1.00   10.00    --  107.94 -30.00 -90.00   53
  3  \w     79.00 123.00   1.00   10.00    --  107.94 -77.00-120.00   44
  4  \w     46.00  98.00   1.00   10.00    --  107.94 -45.00  30.00   52
  5  \w     77.00 116.00   1.00   10.00    --  107.94-111.00  60.00   39
  6  \w     42.00  82.00   1.00    1.95    --   40.81 -99.00 150.00   40
  7  \w     11.00  44.00   1.00    1.95    --   40.81 -99.00  90.00   33
  8  \w     -1.00  34.00   1.00    1.95    --  -40.81  38.00-150.00   35
  9  \w     34.00 114.00   1.00   10.00    --  107.94-111.00-150.00   80
 10  \w     30.00  88.00   1.00   10.00    --  107.94 -30.00-180.00   58
 11  \w    100.00 132.00   1.00   10.00    --  107.94 111.00 -60.00   32
 12  \w    102.00 178.00   1.00   10.00    --  107.94 111.00-180.00   76
 13  \w    -49.00  25.00   1.00    1.95    --  -40.81  38.00-180.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1239003000
_diffrn_orient_matrix_UB_12      -0.0019587000
_diffrn_orient_matrix_UB_13      0.0285960000
_diffrn_orient_matrix_UB_21      0.0251735000
_diffrn_orient_matrix_UB_22      0.0946726000
_diffrn_orient_matrix_UB_23      0.0402284000
_diffrn_orient_matrix_UB_31      -0.0837080000
_diffrn_orient_matrix_UB_32      0.0311704000
_diffrn_orient_matrix_UB_33      -0.1195511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.383
_diffrn_reflns_theta_min         5.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_preparation
'Reaction between 4-hydroxybenzoic acid and magnesium acetate in dioxane at room temperature'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,4-dioxane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0610P)^2^+0.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1688
_reflns_number_total             2008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00163b2.cif
_cod_data_source_block           rs1_mg(hba)diox_sm_abscor
_cod_database_code               7244470
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg C18 H22 O10'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.836
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_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 O(H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.85 with sigma of 0.02
 O3-H3
 0.85 with sigma of 0.02
 H4A-H4B
 1.34 with sigma of 0.04
3.a Free rotating group:
 O4(H4A,H4B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C7(H7), C6(H6)
;
_shelx_res_checksum              72396
_shelx_hkl_checksum              94113
_olex2_exptl_crystal_mounting_method 'on loop using oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.777