An uncoordinated tertiary nitrogen based tricarboxylate calcium network with Lewis acid-base dual catalytic sites for cyanosilylation of aldehydes.
Wang, Ying-Xia; Wang, Hui-Min; Meng, Pan; Song, Dong-Xia; Hou, Juan-Juan; Zhang, Xian-Ming; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1740–1745; doi:10.1039/d0dt03747h

data_7706218
_publ_section_title
;
 An uncoordinated tertiary nitrogen based tricarboxylate calcium network
 with Lewis acid-base dual catalytic sites for cyanosilylation of
 aldehydes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1740
_journal_page_last               1745
_journal_paper_doi               10.1039/d0dt03747h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C86 H70 Ca3 N4 O16'
_chemical_formula_sum            'C86 H70 Ca3 N4 O16'
_chemical_formula_weight         1535.70
_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
_audit_creation_date             2020-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2020-11-21 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                73.111(7)
_cell_angle_beta                 84.390(6)
_cell_angle_gamma                76.799(5)
_cell_formula_units_Z            1
_cell_length_a                   8.7338(5)
_cell_length_b                   12.7784(9)
_cell_length_c                   21.2690(19)
_cell_measurement_reflns_used    3059
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8340
_cell_measurement_theta_min      3.8640
_cell_volume                     2210.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_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     45.00  71.00   1.00   32.99    --   17.96 178.00 -30.00   26
  2  \w     -2.00  86.00   1.00   32.99    --   17.96  57.00-180.00   88
  3  \w     -8.00  87.00   1.00   32.99    --   17.96  38.00  90.00   95
  4  \w    -52.00  43.00   1.00   32.99    --   17.96 -38.00 -90.00   95
  5  \w    -31.00   9.00   1.00   32.99    --  -18.27  57.00-120.00   40
  6  \w    -19.00  21.00   1.00   32.99    --  -18.27-102.00  36.00   40
  7  \w    -24.00   2.00   1.00   32.99    --  -18.27 -99.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0819309000
_diffrn_orient_matrix_UB_12      -0.0229527000
_diffrn_orient_matrix_UB_13      -0.0008696000
_diffrn_orient_matrix_UB_21      0.0053342000
_diffrn_orient_matrix_UB_22      0.0312980000
_diffrn_orient_matrix_UB_23      -0.0333753000
_diffrn_orient_matrix_UB_31      0.0150108000
_diffrn_orient_matrix_UB_32      0.0448774000
_diffrn_orient_matrix_UB_33      0.0100697000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_number            18661
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.617
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9410
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1518P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.2637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5369
_reflns_number_total             9410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03747h2.cif
_cod_data_source_block           20190829-7
_cod_depositor_comments          'Adding full bibliography for 7706218.cif.'
_cod_database_code               7706218
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Ca'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O8-C41B = O8-C41A
 1.25 with sigma of 0.02
 N1B-C41B = N2A-C41A
 1.45 with sigma of 0.02
 C41B-C42B
 1.5 with sigma of 0.02
 N1B-C43B = N1B-C44B = N2A-C44B = N2A-C43A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42A) \\sim Ueq, Uanis(C43B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C44A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43B) = Uanis(C44B)
4. Others
 Fixed Sof: N1B(0.5) N2A(0.5) C41A(0.6) C41B(0.4) C42A(0.6) H42A(0.6)
 H42B(0.6) H42C(0.6) C42B(0.4) H42D(0.4) H42E(0.4) H42F(0.4) C43A(0.6)
 H43A(0.6) H43B(0.6) H43C(0.6) C43B(0.4) H43D(0.4) H43E(0.4) H43F(0.4)
 C44A(0.6) H44A(0.6) H44B(0.6) H44C(0.6) C44B(0.4) H44D(0.4) H44E(0.4) H44F(0.4)
5.a Rotating group:
 O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25),
  C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C38(H38), C39(H39)
5.c Idealised Me refined as rotating group:
 C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F), C43A(H43A,H43B,H43C), C43B(H43D,
 H43E,H43F), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F)
;
_shelx_fab_checksum              30537
_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 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.909