Coordination polymers of a bis-isophthalate bridging ligand with single molecule magnet behaviour of the Co<sup>II</sup> analogue.
Chahine, Ali Y.; Phonsri, Wasinee; Murray, Keith S.; Turner, David R.; Batten, Stuart R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5241–5249; doi:10.1039/c9dt04606b

data_7703832
_publ_section_title
;
 Coordination polymers of a bis-isophthalate bridging ligand with single
 molecule magnet behaviour of the Co<sup>II</sup> analogue.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5241
_journal_page_last               5249
_journal_paper_doi               10.1039/c9dt04606b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C23 H24 N2 O8 Zn, 4.5(H2 O)'
_chemical_formula_sum            'C23 H33 N2 O12.5 Zn'
_chemical_formula_weight         602.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-03-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-14 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8716(4)
_cell_length_b                   9.3173(2)
_cell_length_c                   14.1140(4)
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    123.00(13)
_cell_measurement_theta_max      75.8750
_cell_measurement_theta_min      4.4530
_cell_volume                     2613.20(11)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -58.00  24.00   0.50    1.93    --  -48.53  37.00  60.00  164
  2  \w     43.00  98.00   0.50    1.93    --   48.53-135.00  54.00  110
  3  \w     96.00 124.00   0.50    7.72    --  105.75-135.00  54.00   56
  4  \w     41.00 116.00   0.50    7.72    --  105.75 -61.00 -90.00  150
  5  \w     76.00 107.00   0.50    7.72    --  105.75 -94.00-120.00   62
  6  \w     45.00  75.00   0.50    7.72    --  105.75 -45.00 -90.00   60
  7  \w     36.00  64.00   0.50    7.72    --  105.75 -30.00 -60.00   56
  8  \w     34.00  59.00   0.50    7.72    --  105.75 -45.00   0.00   50
  9  \w     34.00 153.00   0.50    7.72    --  105.75  -2.00  81.00  238
 10  \w     88.00 178.00   0.50    7.72    --  105.75 132.00  32.00  180
 11  \w     36.00  68.00   0.50    7.72    --  105.75 -94.00-120.00   64
 12  \w     36.00 123.00   0.50    7.72    --  105.75-134.00-126.00  174
 13  \w   -120.00  -1.00   0.50    1.93    --  -48.53  -2.00  81.00  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0774380000
_diffrn_orient_matrix_UB_12      -0.0040165000
_diffrn_orient_matrix_UB_13      -0.0045143000
_diffrn_orient_matrix_UB_21      0.0032816000
_diffrn_orient_matrix_UB_22      0.0010332000
_diffrn_orient_matrix_UB_23      -0.1090674000
_diffrn_orient_matrix_UB_31      0.0019343000
_diffrn_orient_matrix_UB_32      -0.1652639000
_diffrn_orient_matrix_UB_33      -0.0005349000
_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  0.0881
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14457
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.239
_diffrn_reflns_theta_min         4.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 1364 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0723P)^2^+4.7594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.610
_reflns_Friedel_fraction_full    0.709
_reflns_Friedel_fraction_max     0.648
_reflns_number_gt                4026
_reflns_number_total             4541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04606b2.cif
_cod_data_source_block           1Zn
_cod_depositor_comments
'Adding full bibliography for 7703831--7703834.cif.'
_cod_original_formula_sum        'C23 H33 N2 O12.50 Zn'
_cod_database_code               7703832
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 C20 H21 N2 O12'
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.597
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O8-H10B
 1.894 with sigma of 0.001
 O4_$2-H9A_$4
 1.963 with sigma of 0.001
 O6-H13B
 2.248 with sigma of 0.001
 H13A-O12
 1.822 with sigma of 0.001
3. Others
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5)
4.a Free rotating group:
 O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C15(H15A,H15B)
4.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C20(H20), C23(H23)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              65394
_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 3.652
_oxdiff_exptl_absorpt_empirical_full_min 0.184