[(Flu)-(CH2)2-(NHC)-CH2-(NHC)-(CH2)2-(Flu)]2-: an ‘all-organic’ hybrid and flexible ligand that enwraps a Ca2+ pseudo-tetrahedrally.
Baguli, Sudip; Das, Shovan; Chakraborty, Mahua; Goswami, Santu; Datta, Ayan; Mukherjee, Debabrata; Chemical Communications  (2022) –; doi:10.1039/D2CC04700D

data_7130823
_publ_section_title
;
 [(Flu)-(CH2)2-(NHC)-CH2-(NHC)-(CH2)2-(Flu)]2-: an
 &#x2018;all-organic&#x2019; hybrid and flexible ligand that enwraps a
 Ca2+ pseudo-tetrahedrally.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04700D
_journal_year                    2022
_chemical_formula_moiety         'C43 H49 Li2 N5 Si2, 2(C7 H8), 1[C7H8]'
_chemical_formula_sum            'C57 H65 Li2 N5 Si2'
_chemical_formula_weight         890.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.11370(10)
_cell_length_b                   30.6579(3)
_cell_length_c                   15.47960(10)
_cell_measurement_reflns_used    32177
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      67.7630
_cell_measurement_theta_min      2.8480
_cell_volume                     5748.82(8)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -73.00  31.00   0.50    1.40    --  -40.33  92.00 -40.00  208
  2  \w    -41.00  26.00   0.50    1.40    --  -40.33  36.00 124.00  134
  3  \w   -107.00 -26.00   0.50    1.40    --  -40.33 -36.00 -31.00  162
  4  \w    -20.00  73.00   0.50    1.40    --   40.33 -92.00-152.00  186
  5  \w     26.00 107.00   0.50    1.40    --   40.33  36.00 124.00  162
  6  \w     19.00  80.00   0.50    1.40    --   40.33-106.00 117.00  122
  7  \w    -83.00 -12.00   0.50    5.60    --  -82.50 106.00-143.00  142
  8  \w   -153.00 -82.00   0.50    5.60    --  -82.50-106.00 117.00  142
  9  \w   -149.00 -68.00   0.50    5.60    --  -82.50 -36.00 -31.00  162
 10  \w     25.00 106.00   0.50    5.60    --   96.67 -92.00-152.00  162
 11  \w     26.00 108.00   0.50    5.60    --   96.67-106.00 117.00  164
 12  \w    104.00 167.00   0.50    5.60    --   96.67 106.00-143.00  126
 13  \w    101.00 168.00   0.50    5.60    --   96.67  92.00 -40.00  134
 14  \w     82.00 163.00   0.50    5.60    --   96.67  36.00 124.00  162
 15  \w    -31.00  30.00   0.50    1.40    --  -40.33  25.00-120.00  122
 16  \w    -26.00  41.00   0.50    1.40    --   40.33 -36.00 -31.00  134
 17  \w    -30.00  31.00   0.50    1.40    --   40.33 -25.00-180.00  122
 18  \w    -47.00 -15.00   0.50    5.60    --  -82.50  42.00-150.00   64
 19  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00-120.00   54
 20  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00 150.00   54
 21  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00 120.00   54
 22  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00 -60.00   54
 23  \w     29.00  68.00   0.50    5.60    --   96.67 -59.00 -30.00   78
 24  \w     29.00  83.00   0.50    5.60    --   96.67 -68.00   0.00  108
 25  \w     29.00  68.00   0.50    5.60    --   96.67 -59.00 -90.00   78
 26  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00 -30.00   54
 27  \w     29.00  83.00   0.50    5.60    --   96.67 -68.00  90.00  108
 28  \w     29.00  83.00   0.50    5.60    --   96.67 -68.00-150.00  108
 29  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00-180.00   54
 30  \w     30.00  57.00   0.50    5.60    --   96.67 -50.00  90.00   54
 31  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00  90.00  192
 32  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00   0.00  192
 33  \w   -108.00 -17.00   0.50    1.40    --  -40.33 -64.00-120.00  182
 34  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00 120.00  192
 35  \w   -108.00 -17.00   0.50    1.40    --  -40.33 -64.00 -60.00  182
 36  \w    -78.00   4.00   0.50    1.40    --  -40.33 104.00  30.00  164
 37  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00  60.00  192
 38  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00-180.00  192
 39  \w    -31.00  30.00   0.50    1.40    --  -40.33  25.00 -30.00  122
 40  \w   -109.00 -13.00   0.50    1.40    --  -40.33 -77.00 -90.00  192
 41  \w     17.00 108.00   0.50    1.40    --   40.33  64.00-120.00  182
 42  \w     17.00 108.00   0.50    1.40    --   40.33  64.00-180.00  182
 43  \w     80.00 163.00   0.50    5.60    --   96.67  42.00  30.00  166
 44  \w     80.00 163.00   0.50    5.60    --   96.67  42.00 -90.00  166
 45  \w     82.00 167.00   0.50    5.60    --   96.67  25.00-150.00  170
 46  \w     75.00 102.00   0.50    5.60    --   96.67  59.00  60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1197629000
_diffrn_orient_matrix_UB_12      0.0161520000
_diffrn_orient_matrix_UB_13      0.0105042000
_diffrn_orient_matrix_UB_21      -0.0278064000
_diffrn_orient_matrix_UB_22      0.0170279000
_diffrn_orient_matrix_UB_23      0.0910437000
_diffrn_orient_matrix_UB_31      0.0327873000
_diffrn_orient_matrix_UB_32      -0.0444167000
_diffrn_orient_matrix_UB_33      0.0387305000
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57785
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.198
_diffrn_reflns_theta_min         3.198
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64262
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 3968 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10110
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+0.6369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                9412
_reflns_number_total             10110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04700d2.cif
_cod_data_source_block           sus_flu2ce_sud2
_cod_database_code               7130823
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Ce Si'
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.635
_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. Rigid body (RIGU) restrains
 C01Q, C01U, C01C, C01O, C01L, C01P, C01X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01H, C01K
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C011(H011)
3.b Secondary CH2 refined with riding coordinates:
 C00Q(H00A,H00B), C00T(H00C,H00D), C00W(H00E,H00H), C00X(H00I,H00J), C014(H01D,
 H01E)
3.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00F(H00F), C00G(H00G), C00K(H00K), C00L(H00L), C00N(H00N),
 C00O(H00O), C00R(H00R), C00S(H00S), C00U(H00U), C00V(H00V), C00Y(H00Y),
 C00Z(H00Z), C012(H012), C013(H013), C015(H015), C016(H016), C017(H017),
 C018(H018), C01A(H01Y), C01C(H1), C01G(H01O), C01H(H01P), C01J(H01T),
 C01K(H01U), C01M(H01Z), C01O(H2), C01P(H3), C01Q(H4), C01U(H5)
3.d Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C01B(H01F,H01G,H01H), C01D(H01I,H01J,H01K), C01E(H01L,
 H01M,H01N), C01I(H01Q,H01R,H01S), C01N(H01V,H01W,H01X), C01T(H01,H,HA),
 C01X(H6,HB,HC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82146
_shelx_hkl_checksum              89928
_shelx_fab_checksum              56172
_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 1.875
_oxdiff_exptl_absorpt_empirical_full_min 0.722