Structural, thermal and topological characterization of coordination networks containing flexible aminocarboxylate ligands with a central biphenylene scaffold
Balestri, Davide; Scilabra, Patrick; Carraro, Claudia; Delledonne, Andrea; Bacchi, Alessia; Mazzeo, Paolo Pio; Carlucci, Lucia; Pelagatti, Paolo; CrystEngComm 21 (2019) 6365–; doi:10.1039/C9CE01230C

data_7233980
_publ_section_title
;
 Structural, thermal and topological characterization of coordination
 networks containing flexible aminocarboxylate ligands with a central
 biphenylene scaffold
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6365
_journal_paper_doi               10.1039/C9CE01230C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '0.5(C74 H78 Cd2 N10 O22), C3 H7 N O'
_chemical_formula_sum            'C40 H46 Cd N6 O12'
_chemical_formula_weight         915.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.46700(10)
_cell_length_b                   16.34960(10)
_cell_length_c                   21.34940(10)
_cell_measurement_reflns_used    50873
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1140
_cell_measurement_theta_min      1.8410
_cell_volume                     4351.66(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 360.00   1.00    1.00   0.00   0.00  -0.00    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0032753000
_diffrn_orient_matrix_UB_12      0.0285089000
_diffrn_orient_matrix_UB_13      0.0243858000
_diffrn_orient_matrix_UB_21      0.0559712000
_diffrn_orient_matrix_UB_22      0.0000565000
_diffrn_orient_matrix_UB_23      -0.0026072000
_diffrn_orient_matrix_UB_31      -0.0030231000
_diffrn_orient_matrix_UB_32      0.0319429000
_diffrn_orient_matrix_UB_33      -0.0217614000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55533
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.944
_diffrn_reflns_theta_min         2.023
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.310
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0203(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4457
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1296P)^2^+6.9104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4251
_reflns_number_total             4457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01230c2.cif
_cod_data_source_block           cd-flex
_cod_depositor_comments
'Adding full bibliography for 7233980--7233983.cif.'
_cod_database_code               7233980
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.947
_reflns_odcompleteness_completeness 87.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.19
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-C16
 1.216 with sigma of 0.02
 N2-C16
 1.363 with sigma of 0.02
 N2-C17
 1.45 with sigma of 0.02
 C18-N2
 1.453 with sigma of 0.02
 O6-N2
 2.298 with sigma of 0.04
 C17-C16
 2.458 with sigma of 0.04
 C18-C17
 2.485 with sigma of 0.04
 N4-C25 \\sim N4-C24
 with sigma of 0.02
3. Rigid bond restraints
 C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.06
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C17 \\sim C18: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C20B) \\sim Ueq, Uanis(C22B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O5) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(C21A)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C20B) \\sim Ueq, Uanis(N3B) \\sim Ueq,
Uanis(C19B) \\sim Ueq, Uanis(C22B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C19A(0.5) H19A(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) N3A(0.5) C19B(0.5) H19B(0.5) C20B(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C22B(0.5) H22A(0.5) H22B(0.5) H22C(0.5) N3B(0.5)
 C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) O6(0.5) C16(0.5) H16(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) N2(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26(0.5) N4(0.5) O7(0.5)
 Fixed X: H17A(0.15457) H17B(0.07098) H17C(0.15025)
 Fixed Y: H17A(0.58089) H17B(0.60046) H17C(0.52672)
 Fixed Z: H17A(0.7433) H17B(0.69053) H17C(0.68277)
6.a Free rotating group:
 O5(C19A,C20A,C21A,N3A), O6(C16,C18,H18A,H18B,H18C,N2)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5), C14(H14), C10(H10), C11(H11), C13(H13), N1(H1),
 C19A(H19A), C19B(H19B), C16(H16), C26(H26)
6.c Fitted hexagon refined as free rotating group:
 C7(C2,C3,C4,C5,C6), C14(C9,C10,C11,C12,C13)
6.d Tetrahedral OH refined with riding coordinates:
 O4(H4)
6.e Idealised Me refined as rotating group:
 C20A(H20D,H20E,H20F), C21A(H21A,H21B,H21C), C20B(H20A,H20B,H20C), C22B(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              46070
_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 1.858
_oxdiff_exptl_absorpt_empirical_full_min 0.629