Fluorenyl-tethered N-heterocyclic carbene (NHC): an exclusive C-donor ligand for heteroleptic calcium and strontium chemistry.
Mondal, Sumana; Sarkar, Subham; Mandal, Chhotan; Mallick, Dibyendu; Mukherjee, Debabrata; Chemical communications (Cambridge, England) 60 (2024) 4553–4556; doi:10.1039/d4cc00397g

data_7132865
_publ_section_title
;
 Fluorenyl-tethered N-heterocyclic carbene (NHC): an exclusive C-donor
 ligand for heteroleptic calcium and strontium chemistry.
;
_journal_issue                   34
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4553
_journal_page_last               4556
_journal_paper_doi               10.1039/d4cc00397g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H47 I N2 O2 Sr, C6 H6'
_chemical_formula_sum            'C44 H53 I N2 O2 Sr'
_chemical_formula_weight         856.40
_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   geom
_audit_creation_date             2024-03-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.13650(10)
_cell_length_b                   21.95920(10)
_cell_length_c                   16.44080(10)
_cell_measurement_reflns_used    33990
_cell_measurement_temperature    100.7(8)
_cell_measurement_theta_max      67.9500
_cell_measurement_theta_min      2.7140
_cell_volume                     3968.10(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.73a 64-bit (release 27-10-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_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     14.00 109.00   0.50    0.20    --   40.58  77.00 120.00  190
  2  \w     14.00 109.00   0.50    0.20    --   40.58  77.00  60.00  190
  3  \w     14.00 109.00   0.50    0.20    --   40.58  77.00   0.00  190
  4  \w     14.00 109.00   0.50    0.20    --   40.58  77.00 -60.00  190
  5  \w     14.00 109.00   0.50    0.20    --   40.58  77.00-180.00  190
  6  \w     18.00 108.00   0.50    0.20    --   40.58  64.00-150.00  180
  7  \w     14.00 109.00   0.50    0.20    --   40.58  77.00-120.00  190
  8  \w     18.00 108.00   0.50    0.20    --   40.58  64.00 150.00  180
  9  \w    105.00 170.00   0.50    0.28    --   96.35  96.00 150.00  130
 10  \w     99.00 160.00   0.50    0.28    --   96.35 117.00 -30.00  122
 11  \w    103.00 164.00   0.50    0.28    --   96.35 108.00 -47.00  122
 12  \w    105.00 170.00   0.50    0.28    --   96.35  96.00-150.00  130
 13  \w     72.00 164.00   0.50    0.28    --   96.35  68.00 -60.00  184
 14  \w     77.00 163.00   0.50    0.28    --   96.35  50.00   0.00  172
 15  \w     72.00 164.00   0.50    0.28    --   96.35  68.00  60.00  184
 16  \w     75.00 165.00   0.50    0.28    --   96.35  59.00  30.00  180
 17  \w     83.00 164.00   0.50    0.28    --   96.35  33.00 120.00  162
 18  \w     71.00 170.00   0.50    0.28    --   96.35  17.00 -90.00  198
 19  \w     41.00 100.00   0.50    0.20    --   40.58-138.00-150.00  118
 20  \w     21.00  79.00   0.50    0.20    --   40.58-108.00-144.00  116
 21  \w     33.00 110.00   0.50    0.28    --   96.35-117.00-180.00  154
 22  \w     29.00 108.00   0.50    0.28    --   96.35-108.00-144.00  158
 23  \w     33.00 110.00   0.50    0.28    --   96.35-117.00  30.00  154
 24  \w     33.00 110.00   0.50    0.28    --   96.35-117.00 -60.00  154
 25  \w     23.00 106.00   0.50    0.28    --   96.35 -96.00 -90.00  166
 26  \w     26.00 127.00   0.50    0.28    --   96.35 -87.00-150.00  202
 27  \w     29.00  83.00   0.50    0.28    --   96.35 -68.00 -60.00  108
 28  \w     30.00  57.00   0.50    0.28    --   96.35 -50.00  60.00   54
 29  \w     28.00  68.00   0.50    0.28    --   96.35 -59.00  30.00   80
 30  \w     28.00  68.00   0.50    0.28    --   96.35 -59.00 -90.00   80
 31  \w     30.00  57.00   0.50    0.28    --   96.35 -50.00-120.00   54
 32  \w    -29.00  31.00   0.50    0.20    --   40.58 -25.00-150.00  120
 33  \w    -35.00  24.00   0.50    0.20    --   40.58 -12.00-120.00  118
 34  \w    -29.00  31.00   0.50    0.20    --   40.58 -25.00 150.00  120
 35  \w   -108.00 -17.00   0.50    0.20    --  -40.58 -64.00   0.00  182
 36  \w   -150.00 -82.00   0.50    0.28    --  -82.50-108.00-144.00  136
 37  \w   -156.00 -83.00   0.50    0.28    --  -82.50 -96.00-150.00  146
 38  \w   -107.00 -25.00   0.50    0.20    --  -40.58 -38.00 -90.00  164
 39  \w   -107.00 -25.00   0.50    0.20    --  -40.58 -38.00  60.00  164
 40  \w    -83.00 -15.00   0.50    0.28    --  -82.50 108.00 -47.00  136
 41  \w    -79.00   1.00   0.50    0.20    --  -40.58 108.00 -47.00  160
 42  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00-180.00   64
 43  \w    -24.00  35.00   0.50    0.20    --  -40.58  12.00-150.00  118
 44  \w    -57.00  26.00   0.50    0.20    --  -40.58  50.00 -90.00  166
 45  \w    -24.00  35.00   0.50    0.20    --  -40.58  12.00-120.00  118
 46  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00  90.00   64
 47  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00 150.00   64
 48  \w    -31.00  30.00   0.50    0.20    --  -40.58  25.00 150.00  122
 49  \w    -24.00  35.00   0.50    0.20    --  -40.58  12.00  90.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.387
_exptl_absorpt_coefficient_mu    8.280
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
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            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0558P)^2^+2.8457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6719
_reflns_number_total             7013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00397g2.cif
_cod_data_source_block           sm-466_a
_cod_depositor_comments
'Adding full bibliography for 7132864--7132867.cif.'
_cod_database_code               7132865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.263
_shelx_estimated_absorpt_t_min   0.052
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C43 \\sim O2-C11
 with sigma of 0.02
 C29-C21 \\sim C29-C45
 with sigma of 0.02
 C21-C43 \\sim C45-C11
 with sigma of 0.02
 O2-C21 \\sim O2-C45
 with sigma of 0.04
 C29-C43 \\sim C29-C11
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C11, C21, C43, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H29C)=Sof(H29D)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H29A)=Sof(H29B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C11(H11A,H11B), C14(H14A,H14B), C17(H17A,H17B),
 C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B), C29(H29A,H29B), C29(H29C,H29D),
  C30(H30A,H30B), C43(H43A,H43B), C45(H45A,H45B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C12(H12), C15(H15), C18(H18), C22(H22), C24(H24), C28(H28),
 C34(H34), C40(H40), C42(H42), C44(H44), C46(H46), C9(H9), C13(H13), C31(H31),
 C33(H33), C35(H35), C39(H39)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              26334
_shelx_hkl_checksum              67136
_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
;