A 2,2’-Bipyridyl Calcium Complex: Synthesis, Structure and Reactivity Studies
Wu, Lingfeng; Wang, Zhenghui; Liu, Yumiao; Chen, Liang; Ren, Wenshan; Dalton Transactions  (2023) –; doi:10.1039/D3DT00301A

data_7712859
_publ_section_title
;
 A 2,2&#x2019;-Bipyridyl Calcium Complex: Synthesis, Structure and
 Reactivity Studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00301A
_journal_year                    2023
_chemical_formula_moiety         'C38 H49 Ca N5 S'
_chemical_formula_sum            'C38 H49 Ca N5 S'
_chemical_formula_weight         647.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2023-01-18 deposited with the CCDC.	2023-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.7740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.59500(10)
_cell_length_b                   17.4079(2)
_cell_length_c                   10.66230(10)
_cell_measurement_reflns_used    13867
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      71.7700
_cell_measurement_theta_min      4.3970
_cell_volume                     1850.56(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -105.00 -17.00   1.00    1.00    --  -35.97 -38.00 -90.00   88
  2  \w    -55.00  33.00   1.00    1.00    --  -35.97  38.00 -90.00   88
  3  \w   -103.00 -19.00   1.00    1.00    --  -35.97 -57.00 120.00   84
  4  \w      4.00  31.00   1.00    1.00    --   35.97  86.00 128.64   27
  5  \w      6.00  75.00   1.00    1.00    --   35.97 -99.00 -90.00   69
  6  \w      8.00  42.00   1.00    1.00    --   35.97  79.00  16.60   34
  7  \w      7.00 107.00   1.00    1.00    --   35.97  19.00-180.00  100
  8  \w     17.00 105.00   1.00    1.00    --   35.97  38.00  60.00   88
  9  \w      3.00  30.00   1.00    1.00    --   35.97  88.00-151.22   27
 10  \w    -31.00  53.00   1.00    1.00    --   35.97 -57.00   0.00   84
 11  \w      3.00  30.00   1.00    1.00    --   35.97  89.00  84.04   27
 12  \w     38.00 109.00   1.00    2.23    --  107.97-112.00 -90.00   71
 13  \w    103.00 176.00   1.00    2.23    --  107.97  77.00  30.00   73
 14  \w     38.00 129.00   1.00    2.23    --  107.97 -30.00   0.00   91
 15  \w     40.00 125.00   1.00    2.23    --  107.97 -45.00  90.00   85
 16  \w     40.00 125.00   1.00    2.23    --  107.97 -45.00 -60.00   85
 17  \w     39.00 106.00   1.00    2.23    --  107.97 -95.00 -60.00   67
 18  \w     40.00 125.00   1.00    2.23    --  107.97 -45.00-150.00   85
 19  \w     39.00 106.00   1.00    2.23    --  107.97 -95.00  90.00   67
 20  \w     39.00 106.00   1.00    2.23    --  107.97 -95.00  30.00   67
 21  \w     38.00 109.00   1.00    2.23    --  107.97-112.00-150.00   71
 22  \w     40.00 135.00   1.00    2.23    --  107.97 -77.00  90.00   95
 23  \w    103.00 176.00   1.00    2.23    --  107.97  77.00   0.00   73
 24  \w     38.00 109.00   1.00    2.23    --  107.97-112.00   0.00   71
 25  \w     39.00 177.00   1.00    2.23    --  107.97   0.00   0.00  138
 26  \w    -88.00  -7.00   1.00    1.00    --  -35.97 126.00 -90.00   81
 27  \w    -55.00  33.00   1.00    1.00    --  -35.97  38.00  90.00   88
 28  \w    -88.00  -7.00   1.00    1.00    --  -35.97 126.00  60.00   81
 29  \w     19.00 103.00   1.00    1.00    --   35.97  57.00-120.00   84
 30  \w    -31.00  53.00   1.00    1.00    --   35.97 -57.00 150.00   84
 31  \w      2.00  29.00   1.00    1.00    --   35.97  90.00 -45.74   27
 32  \w      9.00  42.00   1.00    1.00    --   35.97  78.00-108.11   33
 33  \w     70.00 178.00   1.00    2.23    --  107.97  15.00-180.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0401163000
_diffrn_orient_matrix_UB_12      -0.0771477000
_diffrn_orient_matrix_UB_13      -0.0466132000
_diffrn_orient_matrix_UB_21      -0.0859597000
_diffrn_orient_matrix_UB_22      0.0192586000
_diffrn_orient_matrix_UB_23      -0.1447515000
_diffrn_orient_matrix_UB_31      0.1219476000
_diffrn_orient_matrix_UB_32      0.0389136000
_diffrn_orient_matrix_UB_33      -0.0209217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19450
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         4.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6373
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0853P)^2^+0.9376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                6225
_reflns_number_total             6373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound3
_cod_database_code               7712859
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 S1 Ca1 '
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C37-C36 \\sim C37A-C36
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C37 \\sim C37A \\sim C36: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
C29 \\sim C31 \\sim C30: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H36A)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C36(H36), C36(H36A), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C34(H34), C8(H8), C11(H11), C7(H7), C32(H32), C14(H14), C17(H17),
 C9(H9), C33(H33), C10(H10), C6(H6), C15(H15), C16(H16), C3(H3), C5(H5), C4(H4)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C38(H38A,H38B,
 H38C), C30(H30A,H30B,H30C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C37(H37A,
 H37B,H37C), C37A(H37D,H37E,H37F)
;
_shelx_res_checksum              79247
_shelx_hkl_checksum              14255
_olex2_date_sample_data_collection 2022-10-22
_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 1.480
_oxdiff_exptl_absorpt_empirical_full_min 0.567