Stars and stripes: hexatopic tris(3,2′:6′,3′′-terpyridine) ligands that unexpectedly form one-dimensional coordination polymers
Manfroni, Giacomo; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; CrystEngComm 24 (2022) 491–503; doi:10.1039/D1CE01531A

data_7244014
_publ_section_title
;
 Stars and stripes: hexatopic
 tris(3,2&#x2032;:6&#x2032;,3&#x2032;&#x2032;-terpyridine) ligands that
 unexpectedly form one-dimensional coordination polymers
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              491
_journal_page_last               503
_journal_paper_doi               10.1039/D1CE01531A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C51 H33 N9, 1.75[C3H7NO]'
_chemical_formula_sum            'C56.25 H45.25 N10.75 O1.75'
_chemical_formula_weight         899.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-13 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3991(5)
_cell_length_b                   15.4857(3)
_cell_length_c                   30.0422(5)
_cell_measurement_reflns_used    81610
_cell_measurement_temperature    150
_cell_measurement_theta_max      58.46
_cell_measurement_theta_min      2.56
_cell_volume                     9490.2(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      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.950
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59250
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         58.129
_diffrn_reflns_theta_min         2.559
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.9821
_exptl_absorpt_correction_T_min  0.1407
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0515
_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^)+(0.1005P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5670
_reflns_number_total             9577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01531a2.cif
_cod_data_source_block           mag156_150k
_cod_depositor_comments
'Adding full bibliography for 7244014--7244015.cif.'
_cod_database_code               7244014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C5(H5), C8(H8), C35(H35), C42(H42), C31(H31), C43(H43), C25(H25),
 C11(H11), C18(H18), C33(H33), C38(H38), C2(H2), C14(H14), C50(H50), C1(H1),
 C51(H51), C32(H32), C39(H39), C34(H34), C46(H46), C16(H16), C21(H21), C22(H22),
  C15(H15), C17(H17), C48(H48), C47(H47), C40(H40), C23(H23), C49(H49),
 C41(H41), C24(H24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29028
_shelx_hkl_checksum              18082
_shelx_fab_checksum              74657
_olex2_date_sample_data_collection 2020-10-01
_olex2_date_sample_submission    2020-09-30
_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 MAG156_150K
_olex2_submission_special_instructions 'No special instructions were received'