Multitopic 3,2':6',3''-terpyridine ligands as 4-connecting nodes in two-dimensional 4,4-networks
Manfroni, Giacomo; Spingler, Bernhard; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; CrystEngComm  (2022) –; doi:10.1039/D2CE01130A

data_7245554
_publ_section_title
;
 Multitopic 3,2':6',3''-terpyridine ligands as 4-connecting nodes in
 two-dimensional 4,4-networks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01130A
_journal_year                    2022
_chemical_formula_moiety
'C72 H44 Cu2 F24 N6 O10, 3.6(C6 H4 Cl2), 2(C H Cl3)'
_chemical_formula_sum            'C95.6 H60.4 Cl13.2 Cu2 F24 N6 O10'
_chemical_formula_weight         2504.12
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.874(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9740(4)
_cell_length_b                   24.5642(6)
_cell_length_c                   19.0265(6)
_cell_measurement_reflns_used    91325
_cell_measurement_temperature    130
_cell_measurement_theta_max      56.84
_cell_measurement_theta_min      2.03
_cell_volume                     5576.1(3)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
X-Area X-Red32 1.65.0.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.1234
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         56.819
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    4.547
_exptl_absorpt_correction_T_max  0.5602
_exptl_absorpt_correction_T_min  0.0035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             2509
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.889
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         11193
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.1224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3500P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3685
_refine_ls_wR_factor_ref         0.4112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8115
_reflns_number_total             11193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01130a2.cif
_cod_data_source_block           ma177(4)_130k
_cod_original_formula_sum        'C95.60 H60.40 Cl13.20 Cu2 F24 N6 O10'
_cod_database_code               7245554
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F7-F9 \\sim F7-F8 \\sim F9-F8
 with sigma of 0.04
 C10-F7 \\sim C10-F9 \\sim C10-F8 \\sim C10-C6
 with sigma of 0.02
 C62-C6 \\sim C62-F13 \\sim C62-F15 \\sim C62-F14
 with sigma of 0.02
 F13-F15 \\sim F13-F14 \\sim F15-F14
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C40) = Uanis(C39) = Uanis(C38) = Uanis(C37) = Uanis(C42) = Uanis(C41)
Uiso(C60) = Uiso(C55) = Uiso(C56) = Uiso(C57) = Uiso(C58) = Uiso(C59)
Uanis(C10) = Uanis(C62)
Uanis(F13) = Uanis(F7) = Uanis(F8) = Uanis(F14) = Uanis(F9) = Uanis(F15)
4. Others
 Fixed Sof: Cl1(0.8) Cl8(0.8) F8(0.5) F7(0.5) F9(0.5) C10(0.5) C38(0.8)
 C39(0.8) H39(0.8) C40(0.8) H40(0.8) C41(0.8) H41(0.8) C42(0.8) H42(0.8)
 C37(0.8) Cl11(0.5) Cl3(0.5) C43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5)
 C46(0.5) H46(0.5) C47(0.5) H47(0.5) C48(0.5) Cl7(0.3) C49(0.3) C50(0.3)
 H50(0.3) C51(0.3) H51(0.3) C52(0.3) H52(0.3) C53(0.3) H53(0.3) C54(0.3)
 Cl2(0.3) Cl9(0.2) C55(0.2) C56(0.2) H56(0.2) C57(0.2) H57(0.2) C58(0.2)
 H58(0.2) C59(0.2) H59(0.2) C60(0.2) Cl5(0.2) F13(0.5) F15(0.5) F14(0.5)
 C62(0.5)
5.a Ternary CH refined with riding coordinates:
 C61(H61)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C16(H16), C14(H14), C19(H19), C26(H26), C22(H22), C11(H11),
 C20(H20), C21(H21), C32(H32), C28(H28), C7(H7), C27(H27), C34(H34), C36(H36),
 C2(H2), C33(H33), C35(H35), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
 C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56),
  C57(H57), C58(H58), C59(H59)
5.d Fitted hexagon refined as free rotating group:
 C38(C39,C40,C41,C42,C37), C43(C44,C45,C46,C47,C48), C49(C50,C51,C52,C53,C54),
 C55(C56,C57,C58,C59,C60)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61957
_shelx_hkl_checksum              23747
_olex2_date_sample_data_collection 2021-01-26
_olex2_date_sample_submission    2021-01-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MA177_4_130K
_olex2_submission_special_instructions 'No special instructions were received'