Synthesis and characterization of C2-symmetric bis(carboxamide) pincer ligands
Razuwika, Rufaro; Munro, Orde Q.; New Journal of Chemistry 48 (2024) 4229–4244; doi:10.1039/D3NJ05502G

data_7062989
_publ_section_title
;
 Synthesis and characterization of C2-symmetric bis(carboxamide) pincer
 ligands
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4229
_journal_page_last               4244
_journal_paper_doi               10.1039/D3NJ05502G
_journal_volume                  48
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C25 H17 N5 O2'
_chemical_formula_sum            'C25 H17 N5 O2'
_chemical_formula_weight         419.446
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-21 deposited with the CCDC.	2024-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.4778(2)
_cell_length_b                   16.9420(7)
_cell_length_c                   25.8329(10)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.53
_cell_volume                     1959.76(14)
_computing_cell_refinement       'APEX 3 (Bruker)'
_computing_data_collection       'APEX 3 (Bruker)'
_computing_data_reduction        'SAINT V8.38A (Bruker)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_device_type  'Bruker Venture D8 Photon I CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.9964
_diffrn_reflns_Laue_measured_fraction_max 0.9965
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30705
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9975
_diffrn_reflns_theta_full        28.0000
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.88
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0533 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.9000.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       needle
_exptl_crystal_F_000             872.568
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.1037
_refine_diff_density_min         -0.1135
_refine_diff_density_rms         0.0289
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.3(3)
_refine_ls_d_res_high            0.7503
_refine_ls_d_res_low             7.0835
_refine_ls_goodness_of_fit_ref   1.1112
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1112
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0292
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              34
_reflns_limit_l_min              -33
_reflns_number_gt                4418
_reflns_number_total             4830
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj05502g2.cif
_cod_data_source_block           NSA_Cpd_1c
_cod_depositor_comments
'Adding full bibliography for 7062987--7062991.cif.'
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7062989
_olex2_refinement_description
;
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      cc-pVTZ
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-01-16_17-15-41
;
_olex2_exptl_crystal_mounting_method
'mounted on a MiTeGen 300 um needle loop with Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'