A rare isocyanide derived from an unprecedented neutral yttrium(ii) bis(amide) complex.
Jena, Rashmi; Benner, Florian; Delano, 4th, Francis; Holmes, Daniel; McCracken, John; Demir, Selvan; Odom, Aaron L.; Chemical science 14 (2023) 4257–4264; doi:10.1039/d3sc00171g

data_1568682
_publ_section_title
;
 A rare isocyanide derived from an unprecedented neutral yttrium(ii)
 bis(amide) complex.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              4257
_journal_page_last               4264
_journal_paper_doi               10.1039/d3sc00171g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C72 H100 N2 Y, C4 H8 O'
_chemical_formula_sum            'C76 H108 N2 O Y'
_chemical_formula_weight         1154.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-15 deposited with the CCDC.	2023-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0163(3)
_cell_length_b                   17.0386(3)
_cell_length_c                   22.7773(4)
_cell_measurement_reflns_used    14802
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4650
_cell_measurement_theta_min      3.6150
_cell_volume                     6719.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.938
_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     -4.00  22.00   0.50   12.00    --  -47.36  94.00-133.00   52
  2  \w     17.00  43.00   0.50   12.00    --   47.36 -94.00 115.00   52
  3  \w    -72.00 -46.00   0.50   48.00    --  -91.75  94.00-133.00   52
  4  \w   -159.00 -85.00   0.50   48.00    --  -91.75 -94.00 115.00  148
  5  \w    127.00 153.00   0.50   48.00    --  106.58  94.00-133.00   52
  6  \w     40.00 102.00   0.50   48.00    --  106.58 -94.00 115.00  124
  7  \w    -26.00  26.00   0.50   12.00    --  -47.36  19.00 -30.00  104
  8  \w    -16.00  25.00   0.50   12.00    --  -47.36  19.00-150.00   82
  9  \w    -26.00  10.00   0.50   12.00    --   47.36 -19.00-180.00   72
 10  \w     46.00 120.00   0.50   12.00    --   47.36  19.00 -30.00  148
 11  \w   -162.00-127.00   0.50   48.00    --  -91.75 -77.00  30.00   70
 12  \w    -50.00 -21.00   0.50   48.00    --  -91.75  45.00   0.00   58
 13  \w   -162.00-137.00   0.50   48.00    --  -91.75 -77.00   0.00   50
 14  \w    -47.00 -20.00   0.50   48.00    --  -91.75  45.00  60.00   54
 15  \w    -52.00 -22.00   0.50   48.00    --  -91.75  45.00 150.00   60
 16  \w   -158.00-133.00   0.50   48.00    --  -91.75 -61.00 -90.00   50
 17  \w   -153.00-122.00   0.50   48.00    --  -91.75 -45.00-120.00   62
 18  \w    -72.00 -31.00   0.50   48.00    --  -91.75  61.00-150.00   82
 19  \w     37.00  65.00   0.50   48.00    --  106.58 -61.00 -90.00   56
 20  \w    144.00 178.00   0.50   48.00    --  106.58  45.00 120.00   68
 21  \w     37.00  70.00   0.50   48.00    --  106.58 -61.00-180.00   66
 22  \w    145.00 177.00   0.50   48.00    --  106.58 125.00 -60.00   64
 23  \w     39.00  69.00   0.50   48.00    --  106.58 -61.00 -60.00   60
 24  \w     45.00  70.00   0.50   48.00    --  106.58 -61.00 120.00   50
 25  \w    127.00 177.00   0.50   48.00    --  106.58  61.00-180.00  100
 26  \w     40.00  66.00   0.50   48.00    --  106.58 -61.00 150.00   52
 27  \w    127.00 173.00   0.50   48.00    --  106.58  77.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0253286000
_diffrn_orient_matrix_UB_12      -0.0828540000
_diffrn_orient_matrix_UB_13      0.0244312000
_diffrn_orient_matrix_UB_21      -0.0367281000
_diffrn_orient_matrix_UB_22      0.0132454000
_diffrn_orient_matrix_UB_23      0.0527913000
_diffrn_orient_matrix_UB_31      -0.0769941000
_diffrn_orient_matrix_UB_32      -0.0336392000
_diffrn_orient_matrix_UB_33      -0.0396349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23782
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.963
_diffrn_reflns_theta_min         3.640
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.100a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.059
_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     427
_refine_ls_number_reflns         6674
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0651P)^2^+10.2826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6185
_reflns_number_total             6674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00171g2.cif
_cod_data_source_block           rjii-95
_cod_depositor_comments
'Adding full bibliography for 1568682--1568684.cif.'
_cod_database_code               1568682
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C72H100N2Y
_chemical_oxdiff_usercomment     3-22-21
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.892
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C11-C12 \\sim C12-C13 \\sim C13-C14
 with sigma of 0.02
 O1-C8 \\sim O1-C9
 with sigma of 0.04
 O2-C11 \\sim O2-C14
 with sigma of 0.02
 O2-C12 \\sim O2-C13
 with sigma of 0.04
 C8-C10 \\sim C7-C9
 with sigma of 0.04
 C12-C14 \\sim C11-C13
 with sigma of 0.04
 C7-C8 \\sim C8-C9 \\sim C9-C10
 with sigma of 0.02
 O1-C7 \\sim O1-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1 \\sim C7 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O2, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.25) C7(0.25) H7A(0.25) H7B(0.25) C8(0.25) H8A(0.25) H8B(0.25)
 C9(0.25) H9A(0.25) H9B(0.25) C10(0.25) H10A(0.25) H10B(0.25) O2(0.25)
 C11(0.25) H3A(0.25) H3B(0.25) C12(0.25) H4A(0.25) H4B(0.25) C13(0.25)
 H5A(0.25) H5B(0.25) C14(0.25) H6A(0.25) H6B(0.25)
6.a Free rotating group:
 O1(C7,C8,C9,C10), O2(C11,C12,C13,C14)
6.b Ternary CH refined with riding coordinates:
 C221(H221), C241(H241), C261(H261), C621(H621), C641(H641), C661(H661)
6.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H3A,H3B), C12(H4A,
 H4B), C13(H5A,H5B), C14(H6A,H6B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C23(H23), C25(H25), C63(H63), C65(H65)
6.e Idealised Me refined as rotating group:
 C222(H222,H223,H224), C223(H225,H226,H227), C242(H242,H243,H244), C243(H245,
 H246,H247), C262(H262,H263,H264), C263(H265,H266,H267), C622(H622,H623,H624),
 C623(H625,H626,H627), C642(H642,H643,H644), C643(H645,H646,H647), C662(H662,
 H663,H664), C663(H665,H666,H667)
;
_shelx_res_checksum              47464
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.605