Bioinspired Mo, W and V complexes bearing a highly hydroxyl-functionalized Schiff base ligand
Salonen, Pasi; Peuronen, Anssi; Lehtonen, Ari; Inorganica Chimica Acta 503 (2020) 119414–; doi:10.1016/j.ica.2020.119414

data_1565312
_publ_section_title
;
 Bioinspired Mo, W and V complexes bearing a highly
 hydroxyl-functionalized Schiff base ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119414
_journal_paper_doi               10.1016/j.ica.2020.119414
_journal_volume                  503
_journal_year                    2020
_chemical_formula_moiety         'C38 H56 N2 O10 V2, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H62 N4 O10 V2'
_chemical_formula_weight         884.83
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 109.853(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.5881(5)
_cell_length_b                   11.6102(3)
_cell_length_c                   12.0429(3)
_cell_measurement_reflns_used    3552
_cell_measurement_temperature    119.98(13)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      2.4940
_cell_volume                     2181.51(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     25.00  51.00   1.00    2.50    --  -17.59  77.00-120.00   26
  2  \w    -48.00 -22.00   1.00    2.50    --  -17.59  77.00-120.00   26
  3  \w     -9.00  53.00   1.00    2.50    --   18.69  77.00  90.00   62
  4  \w     -9.00  86.00   1.00    2.50    --   18.69  77.00 -30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0069202000
_diffrn_orient_matrix_UB_12      0.0204205000
_diffrn_orient_matrix_UB_13      0.0515816000
_diffrn_orient_matrix_UB_21      -0.0445464000
_diffrn_orient_matrix_UB_22      0.0042877000
_diffrn_orient_matrix_UB_23      -0.0317132000
_diffrn_orient_matrix_UB_31      -0.0057496000
_diffrn_orient_matrix_UB_32      -0.0573908000
_diffrn_orient_matrix_UB_33      0.0160464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.272
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+1.1643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3926
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-503-119414.cif
_cod_data_source_block           3
_cod_database_code               1565312
_chemical_oxdiff_formula         C38H56N2O10V2
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C)
;