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_1565311
_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         'C19 H31 N O7 W'
_chemical_formula_sum            'C19 H31 N O7 W'
_chemical_formula_weight         569.30
_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                 95.334(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6296(6)
_cell_length_b                   9.2339(2)
_cell_length_c                   11.4363(4)
_cell_measurement_reflns_used    3219
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      4.4910
_cell_volume                     2063.94(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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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    -31.00  65.00   2.00    2.00    --   41.65 -37.00  60.00   48
  2  \w     14.00 110.00   2.00    2.00    --   41.65  57.00-150.00   48
  3  \w     43.00 137.00   2.00    6.00    --  112.00 -45.00-180.00   47
  4  \w     42.00 102.00   2.00    6.00    --  112.00 -45.00  60.00   30
  5  \w    126.00 178.00   2.00    6.00    --  112.00 111.00 150.00   26
  6  \w     86.00 176.00   2.00    6.00    --  112.00  30.00   0.00   45
  7  \w    113.00 149.00   2.00    6.00    --  112.00 178.00-180.00   18
  8  \w     41.00 115.00   2.00    6.00    --  112.00-111.00-120.00   37
  9  \w     75.00 101.00   2.00    6.00    --  112.00 178.00-180.00   13
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240318000
_diffrn_orient_matrix_UB_12      -0.0269193000
_diffrn_orient_matrix_UB_13      0.1225729000
_diffrn_orient_matrix_UB_21      -0.0695182000
_diffrn_orient_matrix_UB_22      -0.0542386000
_diffrn_orient_matrix_UB_23      -0.0571882000
_diffrn_orient_matrix_UB_31      0.0284449000
_diffrn_orient_matrix_UB_32      -0.1554145000
_diffrn_orient_matrix_UB_33      -0.0012157000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7255
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.106
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.723
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.414
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.891
_refine_diff_density_min         -2.027
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0587P)^2^+0.6433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3331
_reflns_number_total             4020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-503-119414.cif
_cod_data_source_block           2
_cod_original_cell_volume        2063.96(11)
_cod_database_code               1565311
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.298
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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, All O(H) groups
2. Restrained distances
 O7-H7B = O7-H7A = O6-H6
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim O5 \\sim O4: within 3A with sigma of 0.001 and sigma for terminal
atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C3(H3), C7(H7)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;