A new bis-phenolate mesoionic carbene ligand for early transition metal chemistry.
Baltrun, Marc; Watt, Fabian A.; Schoch, Roland; Wölper, Christoph; Neuba, Adam G.; Hohloch, Stephan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14611–14625; doi:10.1039/c9dt03099a

data_7700989
_publ_section_title
;
 A new bis-phenolate mesoionic carbene ligand for early transition metal
 chemistry.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14611
_journal_page_last               14625
_journal_paper_doi               10.1039/c9dt03099a
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_sum            'C57 H85 I3 O3'
_chemical_formula_weight         1198.94
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc22hmgp
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-06-11 deposited with the CCDC.    2019-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                117.8960(10)
_cell_angle_beta                 90.6720(10)
_cell_angle_gamma                92.1240(10)
_cell_formula_units_Z            2
_cell_length_a                   6.12470(10)
_cell_length_b                   22.0786(2)
_cell_length_c                   22.7088(2)
_cell_measurement_reflns_used    41807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1820
_cell_measurement_theta_min      2.1820
_cell_volume                     2710.63(6)
_computing_cell_refinement
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'
_computing_data_collection
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'
_computing_data_reduction
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)'
_computing_molecular_graphics    ' Mercury (Macrae et al, 2006)'
_computing_publication_material
;
Oscail (McArdle et al., 2004),
SHELXL-2017/1 (Sheldrick, 2017)
PLATON (Spek, 2009)
OLEX2  (Dolmanov et al., 2009)
;
_computing_structure_refinement
;
Oscail (McArdle et al., 2004),
ShelXle (H\"ubschle et al., 2011)
SHELXL-2017/1 (Sheldrick, 2017)
OLEX2  (Dolmanov et al., 2009)
;
_computing_structure_solution
;
Oscail (McArdle et al., 2004)
SHELXT (Sheldrick, 2015)
OLEX2  (Dolmanov et al., 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
;
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer 
and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48921
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    13.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   1.0
_exptl_transmission_factor_min   0.0
_refine_diff_density_max         1.450
_refine_diff_density_min         -3.365
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.025(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         15680
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0773P)^2^+4.1292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                15145
_reflns_number_total             15680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03099a2.cif
_cod_data_source_block           tt
_cod_depositor_comments
'Adding full bibliography for 7700989--7700996.cif.'
_cod_database_code               7700989
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.068
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              78721