[(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_7130822
_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 Ca N5 Si2'
_chemical_formula_sum            'C43 H49 Ca N5 Si2'
_chemical_formula_weight         732.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-24 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                111.179(2)
_cell_angle_beta                 105.9930(10)
_cell_angle_gamma                97.2430(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5409(2)
_cell_length_b                   15.2405(2)
_cell_length_c                   15.8200(2)
_cell_measurement_reflns_used    17818
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      68.1730
_cell_measurement_theta_min      3.1650
_cell_volume                     1995.57(7)
_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(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_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     21.00 107.00   0.50    1.12    --   40.33  52.00   5.00  172
  2  \w     77.00 163.00   0.50    4.47    --   96.67  52.00   5.00  172
  3  \w    105.00 170.00   0.50    4.47    --   96.67  96.00 -90.00  130
  4  \w    105.00 170.00   0.50    4.47    --   96.67  96.00-150.00  130
  5  \w     99.00 164.00   0.50    4.47    --   96.67 117.00-180.00  130
  6  \w     83.00 164.00   0.50    4.47    --   96.67  33.00 -90.00  162
  7  \w     78.00 163.00   0.50    4.47    --   96.67  50.00 -60.00  170
  8  \w     83.00 164.00   0.50    4.47    --   96.67  33.00-180.00  162
  9  \w     75.00 164.00   0.50    4.47    --   96.67  59.00 -30.00  178
 10  \w     83.00 164.00   0.50    4.47    --   96.67  33.00 120.00  162
 11  \w     83.00 164.00   0.50    4.47    --   96.67  33.00  60.00  162
 12  \w     41.00  99.00   0.50    1.12    --   40.33-138.00 -60.00  116
 13  \w     41.00  99.00   0.50    1.12    --   40.33-138.00   0.00  116
 14  \w     44.00 127.00   0.50    4.47    --   96.67-145.00  90.00  166
 15  \w     44.00 127.00   0.50    4.47    --   96.67-145.00  60.00  166
 16  \w     44.00 127.00   0.50    4.47    --   96.67-145.00 -30.00  166
 17  \w     41.00  99.00   0.50    1.12    --   40.33-138.00-180.00  116
 18  \w     29.00  59.00   0.50    4.47    --   96.67 -52.00-139.00   60
 19  \w     29.00  83.00   0.50    4.47    --   96.67 -68.00 -90.00  108
 20  \w     29.00  68.00   0.50    4.47    --   96.67 -59.00   0.00   78
 21  \w     30.00  57.00   0.50    4.47    --   96.67 -50.00   0.00   54
 22  \w     27.00 127.00   0.50    4.47    --   96.67 -87.00 -30.00  200
 23  \w     30.00  57.00   0.50    4.47    --   96.67 -50.00  90.00   54
 24  \w     29.00  68.00   0.50    4.47    --   96.67 -59.00 120.00   78
 25  \w     28.00 105.00   0.50    4.47    --   96.67 -77.00 120.00  154
 26  \w     30.00 109.00   0.50    4.47    --   96.67-117.00  60.00  158
 27  \w     30.00 109.00   0.50    4.47    --   96.67-117.00 120.00  158
 28  \w     29.00  68.00   0.50    4.47    --   96.67 -59.00 150.00   78
 29  \w     22.00 106.00   0.50    4.47    --   96.67 -96.00 120.00  168
 30  \w     27.00 127.00   0.50    4.47    --   96.67 -87.00-120.00  200
 31  \w     30.00 109.00   0.50    4.47    --   96.67-117.00-120.00  158
 32  \w     29.00  83.00   0.50    4.47    --   96.67 -68.00-180.00  108
 33  \w    -26.00  60.00   0.50    1.12    --   40.33 -52.00-139.00  172
 34  \w    -24.00  35.00   0.50    1.12    --  -40.33  12.00-120.00  118
 35  \w    -30.00  31.00   0.50    1.12    --   40.33 -25.00   0.00  122
 36  \w    -43.00  26.00   0.50    1.12    --  -40.33  38.00 120.00  138
 37  \w    -47.00 -15.00   0.50    4.47    --  -82.50  42.00 150.00   64
 38  \w    -78.00   4.00   0.50    1.12    --  -40.33 104.00 120.00  164
 39  \w    -59.00  27.00   0.50    1.12    --  -40.33  52.00   5.00  172
 40  \w    -47.00 -15.00   0.50    4.47    --  -82.50  42.00-180.00   64
 41  \w    -57.00 -16.00   0.50    4.47    --  -82.50  50.00 -90.00   82
 42  \w    -59.00 -15.00   0.50    4.47    --  -82.50  52.00   5.00   88
 43  \w   -107.00 -21.00   0.50    1.12    --  -40.33 -52.00-139.00  172
 44  \w   -109.00 -13.00   0.50    1.12    --  -40.33 -77.00 -30.00  192
 45  \w   -106.00 -25.00   0.50    1.12    --  -40.33 -38.00 120.00  162
 46  \w   -108.00 -17.00   0.50    1.12    --  -40.33 -64.00 120.00  182
 47  \w   -109.00 -13.00   0.50    1.12    --  -40.33 -77.00  60.00  192
 48  \w   -109.00 -13.00   0.50    1.12    --  -40.33 -77.00-180.00  192
 49  \w   -150.00 -63.00   0.50    4.47    --  -82.50 -52.00-139.00  174
 50  \w   -149.00 -78.00   0.50    4.47    --  -82.50-117.00 -60.00  142
 51  \w   -149.00 -78.00   0.50    4.47    --  -82.50-117.00 -90.00  142
 52  \w   -153.00 -68.00   0.50    4.47    --  -82.50 -25.00 120.00  170
;
_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      -0.1335163000
_diffrn_orient_matrix_UB_12      0.0341856000
_diffrn_orient_matrix_UB_13      0.0264780000
_diffrn_orient_matrix_UB_21      -0.0110429000
_diffrn_orient_matrix_UB_22      0.0552474000
_diffrn_orient_matrix_UB_23      -0.0651837000
_diffrn_orient_matrix_UB_31      -0.1103368000
_diffrn_orient_matrix_UB_32      -0.0912453000
_diffrn_orient_matrix_UB_33      -0.0863163000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27262
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         3.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73988
_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    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0458P)^2^+0.6229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6345
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04700d2.cif
_cod_data_source_block           sud-bisfluca_sud2
_cod_original_cell_volume        1995.57(6)
_cod_database_code               7130822
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Br Ca'
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.733
_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.a Ternary CH refined with riding coordinates:
 C00M(H00M)
2.b Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00R(H00C,H00D), C00X(H00E,H00F), C010(H01A,H01B), C011(H01C,
 H01D)
2.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00L(H00L), C00N(H00N), C00O(H00O), C00Q(H00Q),
 C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00Y(H00Y), C00Z(H00Z),
 C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C019(H019),
 C01C(H01Q), C01E(H01U)
2.d Idealised Me refined as rotating group:
 C017(H01E,H01F,H01G), C01A(H01K,H01L,H01M), C01B(H01N,H01O,H01P), C01D(H01R,
 H01S,H01T), C01F(H01V,H01W,H01X)
;
_shelx_res_checksum              98111
_shelx_hkl_checksum              8938
_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 1.501
_oxdiff_exptl_absorpt_empirical_full_min 0.730