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_7062991
_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, 2(C H4 O)'
_chemical_formula_sum            'C27 H25 N5 O4'
_chemical_formula_weight         483.531
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                76.605(1)
_cell_angle_beta                 78.871(1)
_cell_angle_gamma                78.901(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2743(3)
_cell_length_b                   11.3528(5)
_cell_length_c                   14.9566(5)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.56
_cell_volume                     1164.76(8)
_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      153.00
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9945
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.9964
_diffrn_reflns_Laue_measured_fraction_max 0.9945
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85728
_diffrn_reflns_point_group_measured_fraction_full 0.9964
_diffrn_reflns_point_group_measured_fraction_max 0.9945
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         33.21
_diffrn_reflns_theta_min         2.89
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7102
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0601 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.9514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             508.344
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.2373
_refine_diff_density_min         -0.2323
_refine_diff_density_rms         0.0576
_refine_ls_d_res_high            0.6488
_refine_ls_d_res_low             7.0514
_refine_ls_goodness_of_fit_ref   1.3006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8894
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.3003
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+0.0074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0453
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7062
_reflns_number_total             8894
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj05502g2.cif
_cod_data_source_block           NSA_Cpd_1b
_cod_depositor_comments
'Adding full bibliography for 7062987--7062991.cif.'
_cod_database_code               7062991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Ueq(H2Sb), Ueq(H2Sa), Ueq(H2Sc): fixed at 0.07 with sigma of 0.1
;
_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_13-11-16
;
_olex2_exptl_crystal_mounting_method
'mounted on a nylon cryoloop with Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'