Catalytic Value Addition of Glycerol to Lactic Acid by Chromium Chloride and its Corresponding Pincer Complex
Narjinari, Himani; Dhole, Sunil; Kumar, Akshai; Catalysis Science & Technology  (2025) –; doi:10.1039/D5CY01041A

data_1575972
_publ_section_title
;
 Catalytic Value Addition of Glycerol to Lactic Acid by Chromium Chloride
 and its Corresponding Pincer Complex
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/D5CY01041A
_journal_year                    2025
_chemical_formula_moiety         'C19 H15 Cl3 Cr N3, 1[H2O]'
_chemical_formula_sum            'C19 H17 Cl3 Cr N3 O'
_chemical_formula_weight         461.70
_chemical_name_common            (Ph2NNN)CrCl3
_chemical_name_systematic        (Ph2NNN)CrCl3
_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   geom
_audit_creation_date             2025-07-31
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-31 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.866(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.800(6)
_cell_length_b                   8.357(3)
_cell_length_c                   16.344(6)
_cell_measurement_reflns_used    4626
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.61
_cell_measurement_theta_min      2.57
_cell_volume                     2095.2(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.00
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1150
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24605
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        18.753
_diffrn_reflns_theta_max         18.753
_diffrn_reflns_theta_min         2.056
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.6484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1109 before and 0.0890 after correction.
The Ratio of minimum to maximum transmission is 0.8712.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol + Water'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         1615
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+19.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1228
_reflns_number_total             1615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01041a2.cif
_cod_data_source_block           hn697_224_3_0m_a
_cod_original_cell_volume        2095.2(12)
_cod_database_code               1575972
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57623
_shelx_fab_checksum              62673
_olex2_submission_special_instructions 'No special instructions were received'