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_7062987
_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_formula_moiety         'C25 H17 N5 O2'
_chemical_formula_sum            'C25 H17 N5 O2'
_chemical_formula_weight         419.446
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                 102.656(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7392(4)
_cell_length_b                   14.6766(8)
_cell_length_c                   15.2758(8)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.39
_cell_volume                     1911.70(17)
_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 0.9944
_diffrn_measured_fraction_theta_max 0.9924
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.9944
_diffrn_reflns_Laue_measured_fraction_max 0.9924
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38141
_diffrn_reflns_point_group_measured_fraction_full 0.9944
_diffrn_reflns_point_group_measured_fraction_max 0.9924
_diffrn_reflns_theta_full        32.5000
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         3.07
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0554 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.9498.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             872.568
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.1377
_refine_diff_density_min         -0.1293
_refine_diff_density_rms         0.0359
_refine_ls_d_res_high            0.6484
_refine_ls_d_res_low             6.6448
_refine_ls_goodness_of_fit_ref   1.0885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0885
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0153P)^2^+0.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0410
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6222
_reflns_number_total             7297
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj05502g2.cif
_cod_data_source_block           NSA_Cpd_1a
_cod_depositor_comments
'Adding full bibliography for 7062987--7062991.cif.'
_cod_database_code               7062987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_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_08-02-30
;
_olex2_submission_special_instructions 'No special instructions were received'