Centric and acentric networks using low-symmetry heterotopic carboxylate/pyridyl ligands
Hall, Gregory S.; Angeles, Melissa J.; Hicks, Jamie; Turner, David R.; CrystEngComm 18 (2016) 6614–; doi:10.1039/C6CE01000H

data_7225795
_publ_section_title
;
 Centric and acentric networks using low-symmetry heterotopic
 carboxylate/pyridyl ligands
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6614
_journal_paper_doi               10.1039/C6CE01000H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C28 H24 Cd N6 O4, 1.5(H2 O)'
_chemical_formula_sum            'C28 H27 Cd N6 O5.5'
_chemical_formula_weight         647.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-28 deposited with the CCDC.
2016-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4690(18)
_cell_length_b                   12.4690(18)
_cell_length_c                   17.439(3)
_cell_measurement_reflns_used    54034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.056
_cell_measurement_theta_min      2.008
_cell_volume                     2711.3(7)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54034
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.056
_diffrn_reflns_theta_min         2.008
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
Electron count calculates for 1.5 H2O per formula unit.
Solvent included in UNIT instruction.
Micro analysis shows 0.4 H2O per formula unit.
;
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 1600 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+2.9093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3877
_reflns_number_total             3908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01000h2.cif
_cod_data_source_block           3Cd
_cod_depositor_comments
'Adding full bibliography for 7225789--7225801.cif.'
_cod_original_cell_volume        2711.3(9)
_cod_original_formula_sum        'C28 H27 Cd N6 O5.50'
_cod_database_code               7225795
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.983
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              37637
_shelx_hkl_checksum              91104
_shelx_fab_checksum              98537
_solvent_exptl_crystal_recrystallization_method DMF:H2O