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_7233982
_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         'C85 H68 N8 O15 Zn4, 4(C3 H7 N O)'
_chemical_formula_sum            'C97 H96 N12 O19 Zn4'
_chemical_formula_weight         1995.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 91.120(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5930(6)
_cell_length_b                   45.238(2)
_cell_length_c                   23.3964(11)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.20
_cell_volume                     12267.8(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      120.24
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            86045
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.598
_diffrn_reflns_theta_min         1.974
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1301 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.8296.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.921
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00208(16)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         33962
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+7.8453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24299
_reflns_number_total             33962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01230c2.cif
_cod_data_source_block           zn1
_cod_depositor_comments
'Adding full bibliography for 7233980--7233983.cif.'
_cod_original_cell_volume        12267.7(10)
_cod_database_code               7233982
_shelx_shelxl_version_number     2014/7
_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
2. Restrained distances
 C5AA-C4AA
 -2.3 with sigma of 0.02
 C5AA-C0AA
 -2.3 with sigma of 0.02
3. Rigid bond restraints
 C30, C31, C27A, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39, C40, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, C46, H46, C47, H47, C48, H48, C49, H49, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2AA, C3AA, H3AA, H3AB, H3AC, N9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1AA, C2AA, N9, H2AA, H2AB, H2AC, C3AA, C1AA, H3AA, H3AB, H3AC, H1AA, C5AA,
 N1AA, C0AA, C4AA, O0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C27A \\sim C28A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C39 \\sim C40 \\sim H40 \\sim C41 \\sim C42 \\sim C43 \\sim H43 \\sim C44:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C45 \\sim C46 \\sim H46 \\sim C47 \\sim H47 \\sim C48 \\sim H48 \\sim C49 \\sim
H49 \\sim C50: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2AA \\sim C3AA \\sim H3AA \\sim H3AB \\sim H3AC \\sim N9: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N1AA \\sim C0AA \\sim C4AA \\sim C5AA \\sim O0AA \\sim N9 \\sim C2AA \\sim H2AA
\\sim H2AB \\sim H2AC \\sim C3AA \\sim C1AA \\sim H3AA \\sim H3AB \\sim H3AC
\\sim O1AA \\sim H1AA: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(N9) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, : with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C3AA)
\\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C5AA) \\sim Ueq, Uanis(N1AA) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(O0AA) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1AA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: H30(0.5) H31A(0.5) H31(0.5) H35A(0.5) H35(0.5) H4A(0.5) C26B(0.5)
 C27B(0.5) H27B(0.5) C28B(0.5) H28B(0.5) C29B(0.5) C36B(0.5) H36B(0.5)
 C37B(0.5) H37B(0.5) C38B(0.5) N7A(0.5) H7A(0.5) C26A(0.5) C29A(0.5) C36A(0.5)
 H36A(0.5) C37A(0.5) H37A(0.5) C38A(0.5) N7B(0.5) H7B(0.5) C2AA(0.5) H2AA(0.5)
 H2AB(0.5) H2AC(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) N9(0.5) N1AA(0.5)
 C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) O1AA(0.5)
 C4AA(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5AA(0.5) H5AA(0.5) O0AA(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C10(H10), C12(H12), C11(H11), C9(H9), C17(H17), C18(H18),
 C16(H16), C15(H15), C22(H22), C24(H24), C23(H23), C21(H21), C30(H30),
 C31(H31A), C31(H31), C34(H34), C35(H35A), C35(H35), C40(H40), C41(H41),
 C43(H43), C42(H42), C48(H48), C46(H46), C47(H47), C49(H49), C52(H52), C53(H53),
  C55(H55), C54(H54), C60(H60), C62(H62), C63(H63), C61(H61), C69(H69),
 C68(H68), C66(H66), C67(H67), C74(H74), C75(H75), C73(H73), C72(H72), C78(H78),
  C79(H79), C81(H81), C80(H80), N3(H3), N4(H4A), N5(H5), N6(H6), N8(H8),
 C27B(H27B), C28B(H28B), C36B(H36B), C37B(H37B), N7A(H7A), C27A(H27A),
 C28A(H28A), C36A(H36A), C37A(H37A), N7B(H7B), C1S(H1S), C4S(H4S), C7S(H7S),
 C1AA(H1AA), C5AA(H5AA)
6.b Fitted hexagon refined as free rotating group:
 C10(C13,C12,C11,C8,C9), C17(C18,C19,C16,C15,C14), C22(C25,C24,C23,C20,C21),
 C39(C40,C41,C44,C43,C42), C48(C45,C46,C47,C50,C49), C51(C52,C53,C56,C55,C54),
 C60(C59,C62,C63,C64,C61), C69(C68,C65,C66,C67,C70), C74(C75,C76,C73,C72,C71),
 C77(C78,C79,C82,C81,C80)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C2AA(H2AA,
 H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC),
 C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,H8SC), C9S(H9SA,H9SB,
 H9SC), C0AA(H0AA,H0AB,H0AC), C4AA(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              27957
_shelx_fab_checksum              24593
_olex2_submission_special_instructions 'No special instructions were received'