[(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_7130821
_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         'C37 H31 Ca N4, 2(C6 H6)'
_chemical_formula_sum            'C49 H43 Ca N4'
_chemical_formula_weight         727.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 104.1130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9502(2)
_cell_length_b                   9.61450(10)
_cell_length_c                   21.1384(2)
_cell_measurement_reflns_used    19368
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      68.1150
_cell_measurement_theta_min      2.8080
_cell_volume                     3735.10(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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     82.00 158.00   0.50    1.14    --   96.67  25.00 -60.00  152
  2  \w    131.00 158.00   0.50    1.14    --   96.67  33.00  60.00   54
  3  \w     96.00 127.00   0.50    1.14    --   96.67  33.00  60.00   62
  4  \w    -24.00  35.00   0.50    0.29    --  -40.33  12.00 150.00  118
  5  \w    -67.00  28.00   0.50    0.29    --  -40.33  77.00  60.00  190
  6  \w    -24.00  35.00   0.50    0.29    --  -40.33  12.00 -90.00  118
  7  \w    -31.00  30.00   0.50    0.29    --  -40.33  25.00 -90.00  122
  8  \w    -24.00  35.00   0.50    0.29    --  -40.33  12.00 -30.00  118
  9  \w    104.00 169.00   0.50    1.14    --   96.67  94.00 -34.00  130
 10  \w     81.00 158.00   0.50    1.14    --   96.67 145.00 -90.00  154
 11  \w     99.00 164.00   0.50    1.14    --   96.67 117.00 -60.00  130
 12  \w    -35.00  24.00   0.50    0.29    --   40.33 -12.00 -60.00  118
 13  \w     40.00  79.00   0.50    1.14    --   96.67 -68.00-120.00   78
 14  \w     37.00  62.00   0.50    1.14    --   96.67 -59.00-150.00   50
 15  \w     28.00 105.00   0.50    1.14    --   96.67 -77.00-150.00  154
 16  \w     41.00  68.00   0.50    1.14    --   96.67 -59.00 -60.00   54
 17  \w     31.00  57.00   0.50    1.14    --   96.67 -50.00 -90.00   52
 18  \w     30.00  55.00   0.50    1.14    --   96.67 -50.00 -30.00   50
 19  \w     33.00  80.00   0.50    1.14    --   96.67 -68.00   0.00   94
 20  \w     41.00  68.00   0.50    1.14    --   96.67 -59.00  60.00   54
 21  \w     30.00  56.00   0.50    1.14    --   96.67 -50.00  90.00   52
 22  \w     30.00  57.00   0.50    1.14    --   96.67 -50.00  60.00   54
 23  \w    -26.00  43.00   0.50    0.29    --   40.33 -38.00 150.00  138
 24  \w     32.00  57.00   0.50    1.14    --   96.67 -50.00  30.00   50
 25  \w     30.00  55.00   0.50    1.14    --   96.67 -50.00-120.00   50
 26  \w     24.00 107.00   0.50    1.14    --   96.67 -94.00-145.00  166
 27  \w     68.00  94.00   0.50    1.14    --   96.67-117.00 -30.00   52
 28  \w     32.00  63.00   0.50    1.14    --   96.67-117.00 -30.00   62
 29  \w     30.00  56.00   0.50    1.14    --   96.67-117.00   0.00   52
 30  \w     65.00 106.00   0.50    1.14    --   96.67-117.00   0.00   82
 31  \w     18.00  79.00   0.50    0.29    --   40.33-104.00  30.00  122
 32  \w    -13.00  73.00   0.50    0.29    --   40.33 -94.00-145.00  172
 33  \w    -47.00 -15.00   0.50    1.14    --  -82.50  42.00  90.00   64
 34  \w    -47.00 -15.00   0.50    1.14    --  -82.50  42.00 120.00   64
 35  \w    -47.00 -15.00   0.50    1.14    --  -82.50  42.00  60.00   64
 36  \w    -74.00  32.00   0.50    0.29    --  -40.33  94.00 -34.00  212
 37  \w    -81.00 -10.00   0.50    1.14    --  -82.50  94.00 -34.00  142
 38  \w   -153.00 -68.00   0.50    1.14    --  -82.50 -25.00 -90.00  170
 39  \w   -157.00 -83.00   0.50    1.14    --  -82.50 -96.00  30.00  148
 40  \w   -155.00 -82.00   0.50    1.14    --  -82.50 -94.00-145.00  146
;
_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      0.0823547000
_diffrn_orient_matrix_UB_12      0.0006286000
_diffrn_orient_matrix_UB_13      0.0317369000
_diffrn_orient_matrix_UB_21      -0.0056379000
_diffrn_orient_matrix_UB_22      -0.1484471000
_diffrn_orient_matrix_UB_23      0.0257536000
_diffrn_orient_matrix_UB_31      0.0147480000
_diffrn_orient_matrix_UB_32      -0.0602385000
_diffrn_orient_matrix_UB_33      -0.0630546000
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.230
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93158
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00053(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.2392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6281
_reflns_number_total             6796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04700d2.cif
_cod_data_source_block           sud-bisfluca2_sud1
_cod_database_code               7130821
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N H Ca Si'
_chemical_oxdiff_usercomment     100k
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C015(H015)
2.b Secondary CH2 refined with riding coordinates:
 C00K(H00A,H00B), C00N(H00C,H00E), C00R(H00G,H00K), C00V(H00N,H00O), C00W(H00R,
 H00V)
2.c Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I), C00J(H00J), C00L(H00L),
 C00M(H00M), C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013),
 C014(H014), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A),
 C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G),
 C01H(H01H), C01I(H01I)
;
_shelx_res_checksum              8275
_shelx_hkl_checksum              89861
_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.726