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_7132867
_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         'C35.994 H48.981 Ca N3 Si2'
_chemical_formula_sum            'C35.99 H48.98 Ca N3 Si2'
_chemical_formula_weight         619.94
_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   geom
_audit_creation_date             2024-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.8930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9451(2)
_cell_length_b                   9.60320(10)
_cell_length_c                   35.7576(3)
_cell_measurement_reflns_used    22452
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      68.0860
_cell_measurement_theta_min      2.5730
_cell_volume                     7247.62(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_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    -24.00  35.00   0.50    0.48    --  -40.33  12.00 -30.00  118
  2  \w    -31.00  30.00   0.50    0.48    --  -40.33  25.00 -90.00  122
  3  \w    -31.00  30.00   0.50    0.48    --  -40.33  25.00  60.00  122
  4  \w    -47.00 -15.00   0.50    2.40    --  -82.50  42.00  30.00   64
  5  \w    -47.00 -15.00   0.50    2.40    --  -82.50  42.00 -60.00   64
  6  \w   -108.00 -15.00   0.50    0.48    --  -40.33 -71.00  14.00  186
  7  \w    -28.00  66.00   0.50    0.48    --   40.33 -71.00  14.00  188
  8  \w     41.00  99.00   0.50    0.48    --   40.33-138.00 -60.00  116
  9  \w     41.00  99.00   0.50    0.48    --   40.33-138.00-180.00  116
 10  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00-180.00   54
 11  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00-150.00   54
 12  \w     82.00 167.00   0.50    2.40    --   96.67  25.00-120.00  170
 13  \w     82.00 167.00   0.50    2.40    --   96.67  25.00 -60.00  170
 14  \w    105.00 170.00   0.50    2.40    --   96.67  96.00  60.00  130
 15  \w     81.00 164.00   0.50    2.40    --   96.67 145.00  90.00  166
 16  \w     80.00 163.00   0.50    2.40    --   96.67  42.00 120.00  166
 17  \w     72.00 165.00   0.50    2.40    --   96.67  71.00 145.00  186
 18  \w     29.00  89.00   0.50    2.40    --   96.67 -71.00  14.00  120
 19  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00  30.00   54
 20  \w     29.00  68.00   0.50    2.40    --   96.67 -59.00   0.00   78
 21  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00  60.00   54
 22  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00  90.00   54
 23  \w     29.00  68.00   0.50    2.40    --   96.67 -59.00 120.00   78
 24  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00 150.00   54
 25  \w     29.00  83.00   0.50    2.40    --   96.67 -68.00  90.00  108
 26  \w     30.00  57.00   0.50    2.40    --   96.67 -50.00   0.00   54
 27  \w     29.00  83.00   0.50    2.40    --   96.67 -68.00  60.00  108
 28  \w     30.00 109.00   0.50    2.40    --   96.67-117.00  30.00  158
 29  \w     78.00 163.00   0.50    2.40    --   96.67  50.00-120.00  170
 30  \w     15.00 109.00   0.50    0.48    --   40.33  71.00 145.00  188
 31  \w    -35.00  24.00   0.50    0.48    --   40.33 -12.00  60.00  118
 32  \w    -65.00  28.00   0.50    0.48    --  -40.33  71.00 145.00  186
 33  \w    -89.00 -14.00   0.50    2.40    --  -82.50  71.00 145.00  150
 34  \w   -151.00 -57.00   0.50    2.40    --  -82.50 -71.00  14.00  188
 35  \w    -35.00  24.00   0.50    0.48    --   40.33 -12.00-180.00  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  0.0286
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            27194
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.179
_diffrn_reflns_theta_min         2.570
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0431P)^2^+13.3262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6373
_reflns_number_total             6559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00397g2.cif
_cod_data_source_block           sm-111d
_cod_depositor_comments
'Adding full bibliography for 7132864--7132867.cif.'
_cod_database_code               7132867
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.498
_olex2_refinement_description
;
1. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Fixed Sof: Ca1(0.97) Ca2(0.03)
2.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C15(H15), C18(H18), C14(H14), C11(H11), C16(H16), C12(H12),
 C17(H17), C13(H13), C21(H21), C23(H23), C22(H22)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C33(H33A,
 H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              58649
_shelx_hkl_checksum              17394
_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
;