Quinolino[7,8-h]quinoline: A ‘Just Right’ Ligand for Beryllium(II) Coordination
Buchanan, Jenna; Severinsen, Rebecca; Buchner, Magnus Richard; Thomas-Hargreaves, Lewis; Spang, Nils; John, Kevin; Plieger, Paul; Dalton Transactions  (2021) –; doi:10.1039/D1DT03367K

data_7708818
_publ_section_title
;
 Quinolino[7,8-h]quinoline: A &#x2018;Just Right&#x2019; Ligand for
 Beryllium(II) Coordination
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03367K
_journal_year                    2021
_chemical_formula_moiety         'C18 H13 Be Br N3 O2, C2 H3 N, Br'
_chemical_formula_sum            'C20 H16 Be Br2 N4 O2'
_chemical_formula_weight         513.20
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3825(3)
_cell_length_b                   9.6565(2)
_cell_length_c                   19.2412(5)
_cell_measurement_reflns_used    42193
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.76
_cell_measurement_theta_min      4.13
_cell_volume                     2054.77(9)
_computing_cell_refinement
;
X-Area Recipe 1.36 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3 (STOE, 2020)
X-Area LANA 1.83.8(STOE, 2020)
;
_computing_molecular_graphics    'Diamond v4.6.6 (Brandenburg, 2021)'
_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 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      ' 3987 frames, detector distance = 67 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_unetI/netI     0.0069
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24275
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         78.717
_diffrn_reflns_theta_min         4.135
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  0.5472
_exptl_absorpt_correction_T_min  0.2405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0192
_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^)+(0.0250P)^2^+1.4071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             4331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03367k2.cif
_cod_data_source_block           NSP023
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7708818
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.509
_shelx_estimated_absorpt_t_max   0.509
_shelx_res_checksum              94416
_shelx_hkl_checksum              50517