A mesoionic nitrogen-donor ligand: structure, iridium coordination, and catalytic effects.
Navarro, Miquel; Li, Mo; Bernhard, Stefan; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 659–662; doi:10.1039/c7dt04555g

data_7044970
_publ_section_title
;
 A mesoionic nitrogen-donor ligand: structure, iridium coordination, and
 catalytic effects.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              659
_journal_page_last               662
_journal_paper_doi               10.1039/c7dt04555g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '4(C16 H18 N2 O4), 4(H2 O), 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H84 Cl4 N8 O20'
_chemical_formula_weight         1451.21
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2017-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.969(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.6020(2)
_cell_length_b                   13.05540(10)
_cell_length_c                   12.1795(2)
_cell_measurement_reflns_used    11721
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      27.4530
_cell_measurement_theta_min      2.1020
_cell_volume                     1754.83(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     35.00 122.00   1.00    5.58    --   27.42 178.00  30.00   87
  2  \w    -10.00 103.00   1.00    5.58    --   27.42  57.00 -60.00  113
  3  \w     35.00 122.00   1.00    5.58    --   27.42 178.00-150.00   87
  4  \w     35.00 122.00   1.00    5.58    --   27.42 178.00 120.00   87
  5  \w    -57.00 114.00   1.00    5.58    --   27.42  19.00  60.00  171
  6  \w    -49.00  65.00   1.00    5.58    --   27.42 -57.00 150.00  114
  7  \w    -20.00  32.00   1.00    5.58    --  -23.50 -99.00 -30.00   52
  8  \w    -10.00 103.00   1.00    5.58    --   27.42  57.00-120.00  113
  9  \w    -16.00 112.00   1.00    5.58    --   27.42  77.00  60.00  128
 10  \w    -49.00   4.00   1.00    5.58    --   27.42 -57.00   0.00   53
 11  \w    -10.00 103.00   1.00    5.58    --   27.42  57.00 150.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0366823000
_diffrn_orient_matrix_UB_12      -0.0226181000
_diffrn_orient_matrix_UB_13      -0.0519999000
_diffrn_orient_matrix_UB_21      0.0031560000
_diffrn_orient_matrix_UB_22      -0.0477012000
_diffrn_orient_matrix_UB_23      0.0286713000
_diffrn_orient_matrix_UB_31      -0.0526886000
_diffrn_orient_matrix_UB_32      0.0128739000
_diffrn_orient_matrix_UB_33      0.0148626000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25283
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0441P)^2^+0.4867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             3089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04555g2.cif
_cod_data_source_block           17ma118
_cod_depositor_comments
'Adding full bibliography for 7044968--7044970.cif.'
_cod_database_code               7044970
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C16H18N2O4
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.930
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Fixed Sof: O1WB(0.5) H1WA(0.5) H1WB(0.5) Cl2(0.25) Cl3(0.25) C2(0.25)
 H2A(0.25) H2B(0.25) Cl1(0.25) Cl4(0.25) C8(0.25) H8A(0.25) H8B(0.25) O1WA(0.5)
 H1WC(0.5) H1WD(0.5)
 Fixed Uiso: H1WA(0.064) H1WB(0.064) H2A(0.11) H2B(0.11) H8A(0.067) H8B(0.067)
 H1WC(0.077) H1WD(0.077)
 Fixed X: H1WA(0.63389) H1WB(0.5505) H2A(1.10051) H2B(0.96952) H8A(1.06616)
 H8B(1.131781) H1WC(1.04781) H1WD(1.14809)
 Fixed Y: H1WA(0.20032) H1WB(0.17098) H2A(0.527841) H2B(0.54692) H8A(0.444468)
 H8B(0.482759) H1WC(0.33352) H1WD(0.29891)
 Fixed Z: H1WA(0.30364) H1WB(0.20511) H2A(1.09989) H2B(1.10692) H8A(0.930459)
 H8B(1.05706) H1WC(0.72341) H1WD(0.80335)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C7(H7), C22(H22), C3(H3), C5(H5), C4(H4)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              5081
_olex2_date_sample_data_collection 2017-08-24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.813