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_7712858
_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         'C35 H50 Ca N5 O'
_chemical_formula_sum            'C35 H50 Ca N5 O'
_chemical_formula_weight         596.88
_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             2022-08-30
_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                78.478(6)
_cell_angle_beta                 81.896(6)
_cell_angle_gamma                67.135(7)
_cell_formula_units_Z            2
_cell_length_a                   10.2949(7)
_cell_length_b                   10.3859(8)
_cell_length_c                   17.1736(12)
_cell_measurement_reflns_used    8735
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      72.8910
_cell_measurement_theta_min      4.5990
_cell_volume                     1653.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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 -21.00   1.00    4.58    --  -37.54 -57.00-150.00   84
  2  \w    -64.00  30.00   1.00    4.58    --  -37.54  77.00-150.00   94
  3  \w   -105.00 -11.00   1.00    4.58    --  -37.54 -77.00  90.00   94
  4  \w    -54.00  30.00   1.00    4.58    --  -37.54  57.00   0.00   84
  5  \w     11.00 105.00   1.00    4.58    --   37.54  77.00  30.00   94
  6  \w     19.00 107.00   1.00    4.58    --   37.54  38.00 -90.00   88
  7  \w     24.00  92.00   1.00    4.58    --   37.54-126.00   0.00   68
  8  \w     21.00 105.00   1.00    4.58    --   37.54  57.00 -90.00   84
  9  \w    -32.00  56.00   1.00    4.58    --   37.54 -38.00 -60.00   88
 10  \w      8.00 109.00   1.00    4.58    --   37.54  19.00 150.00  101
 11  \w    -34.00  67.00   1.00    4.58    --   37.54 -19.00 150.00  101
 12  \w     21.00 105.00   1.00    4.58    --   37.54  57.00 150.00   84
 13  \w     24.00  92.00   1.00    4.58    --   37.54-126.00  60.00   68
 14  \w    -32.00  56.00   1.00    4.58    --   37.54 -38.00 120.00   88
 15  \w    -32.00  56.00   1.00    4.58    --   37.54 -38.00 -30.00   88
 16  \w     19.00 107.00   1.00    4.58    --   37.54  38.00 -60.00   88
 17  \w     21.00 105.00   1.00    4.58    --   37.54  57.00-150.00   84
 18  \w     24.00  92.00   1.00    4.58    --   37.54-126.00-180.00   68
 19  \w    -32.00  56.00   1.00    4.58    --   37.54 -38.00-120.00   88
 20  \w     24.00  92.00   1.00    4.58    --   37.54-126.00  90.00   68
 21  \w    -32.00  56.00   1.00    4.58    --   37.54 -38.00   0.00   88
 22  \w     41.00 109.00   1.00   18.32    --  110.47 -95.00  30.00   68
 23  \w     93.00 178.00   1.00   18.32    --  110.47  45.00-150.00   85
 24  \w     41.00 109.00   1.00   18.32    --  110.47 -95.00 -30.00   68
 25  \w     89.00 178.00   1.00   18.32    --  110.47  30.00 -60.00   89
 26  \w     92.00 177.00   1.00   18.32    --  110.47  61.00 120.00   85
 27  \w     44.00 129.00   1.00   18.32    --  110.47 -61.00 120.00   85
 28  \w     89.00 178.00   1.00   18.32    --  110.47  30.00-180.00   89
 29  \w     41.00 116.00   1.00   18.32    --  110.47-112.00 120.00   75
 30  \w     41.00 109.00   1.00   18.32    --  110.47 -95.00 150.00   68
 31  \w     41.00 109.00   1.00   18.32    --  110.47 -95.00-120.00   68
 32  \w     41.00 116.00   1.00   18.32    --  110.47-112.00  30.00   75
 33  \w    101.00 178.00   1.00   18.32    --  110.47 112.00 150.00   77
 34  \w     44.00 129.00   1.00   18.32    --  110.47 -61.00  90.00   85
 35  \w     89.00 178.00   1.00   18.32    --  110.47  30.00 -90.00   89
 36  \w     57.00 151.00   1.00   18.32    --  110.47 178.00  30.00   94
 37  \w     42.00 128.00   1.00   18.32    --  110.47 -45.00   0.00   86
 38  \w     44.00 129.00   1.00   18.32    --  110.47 -61.00-150.00   85
 39  \w    -54.00  30.00   1.00    4.58    --  -37.54  57.00 150.00   84
 40  \w     11.00 105.00   1.00    4.58    --   37.54  77.00-120.00   94
 41  \w     11.00 105.00   1.00    4.58    --   37.54  77.00 150.00   94
 42  \w     11.00 105.00   1.00    4.58    --   37.54  77.00 -90.00   94
 43  \w     11.00 105.00   1.00    4.58    --   37.54  77.00 -30.00   94
;
_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      -0.0642862000
_diffrn_orient_matrix_UB_12      0.1482096000
_diffrn_orient_matrix_UB_13      -0.0494584000
_diffrn_orient_matrix_UB_21      -0.1286254000
_diffrn_orient_matrix_UB_22      0.0366031000
_diffrn_orient_matrix_UB_23      0.0610355000
_diffrn_orient_matrix_UB_31      0.0763459000
_diffrn_orient_matrix_UB_32      0.0572803000
_diffrn_orient_matrix_UB_33      0.0474500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.988
_diffrn_reflns_theta_min         4.673
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6473
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0830P)^2^+0.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5314
_reflns_number_total             6473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        1653.7(2)
_cod_database_code               7712858
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 O1 Ca1'
_reflns_odcompleteness_completeness 99.93
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-C32 \\sim C34A-C33 \\sim C34-C33 \\sim C35-C34A \\sim C35-C34
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(H35C)=Sof(H35D)=Sof(H33C)=Sof(H33D)=Sof(C34)=Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(H35A)=Sof(H35B)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C20(H20), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C35(H35A,H35B), C35(H35C,H35D), C32(H32A,
 H32B), C33(H33A,H33B), C33(H33C,H33D), C34A(H34A,H34B), C34(H34C,H34D)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C1(H1), C7(H7), C18(H18), C8(H8), C17(H17), C16(H16), C4(H4),
 C10(H10), C9(H9), C3(H3), C2(H2)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 2017-12-08
_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 12.701
_oxdiff_exptl_absorpt_empirical_full_min 0.553