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_7712864
_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         'C44 H50 Ca N5 O, 2(C4 H8 O)'
_chemical_formula_sum            'C52 H66 Ca N5 O3'
_chemical_formula_weight         849.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-29
_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                 95.7924(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.30148(10)
_cell_length_b                   20.12994(16)
_cell_length_c                   18.18427(15)
_cell_measurement_reflns_used    20931
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      71.7740
_cell_measurement_theta_min      4.5020
_cell_volume                     4844.12(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      180.01(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 0.986
_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    1.13    --  -35.97 -38.00 -90.00   88
  2  \w   -103.00 -19.00   1.00    1.13    --  -35.97 -57.00 -60.00   84
  3  \w   -103.00 -19.00   1.00    1.13    --  -35.97 -57.00-180.00   84
  4  \w    -53.00  31.00   1.00    1.13    --  -35.97  57.00  90.00   84
  5  \w    -90.00  -3.00   1.00    1.13    --  -35.97 126.00 -90.00   87
  6  \w     24.00  90.00   1.00    1.13    --   35.97-126.00-120.00   66
  7  \w     40.00 125.00   1.00    4.52    --  107.97 -45.00-150.00   85
  8  \w     39.00 110.00   1.00    4.52    --  107.97 -95.00  30.00   71
  9  \w     40.00 125.00   1.00    4.52    --  107.97 -45.00  30.00   85
 10  \w     40.00 125.00   1.00    4.52    --  107.97 -45.00 150.00   85
 11  \w     91.00 176.00   1.00    4.52    --  107.97  45.00-180.00   85
 12  \w     57.00 150.00   1.00    4.52    --  107.97 178.00  90.00   93
 13  \w     38.00 112.00   1.00    4.52    --  107.97-112.00-150.00   74
 14  \w     90.00 175.00   1.00    4.52    --  107.97  61.00 -90.00   85
 15  \w     41.00 126.00   1.00    4.52    --  107.97 -61.00 -30.00   85
 16  \w   -103.00 -19.00   1.00    1.13    --  -35.97 -57.00  60.00   84
 17  \w   -103.00 -19.00   1.00    1.13    --  -35.97 -57.00 120.00   84
 18  \w   -103.00 -19.00   1.00    1.13    --  -35.97 -57.00   0.00   84
 19  \w    -53.00  31.00   1.00    1.13    --  -35.97  57.00-150.00   84
 20  \w     70.00 178.00   1.00    4.52    --  107.97  15.00  30.00  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      -0.1060110000
_diffrn_orient_matrix_UB_12      -0.0119923000
_diffrn_orient_matrix_UB_13      0.0246252000
_diffrn_orient_matrix_UB_21      0.0218864000
_diffrn_orient_matrix_UB_22      -0.0751037000
_diffrn_orient_matrix_UB_23      0.0055255000
_diffrn_orient_matrix_UB_31      0.0429084000
_diffrn_orient_matrix_UB_32      0.0087726000
_diffrn_orient_matrix_UB_33      0.0812720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36395
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.856
_diffrn_reflns_theta_min         3.998
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       plate
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9379
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0860P)^2^+3.1950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8711
_reflns_number_total             9379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound5
_cod_database_code               7712864
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 Ca1 O1'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.758
_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
 C50-C49 \\sim C50-C51 \\sim C51A-C50 \\sim C51-C52 \\sim C52A-C51A
 with sigma of 0.001
 O3-C52A \\sim O3-C49
 with sigma of 0.001
 C47-C48 \\sim C47-C46 \\sim C45-C46
 with sigma of 0.001
 O2-C48 \\sim O2-C45
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51 \\sim C51A \\sim C52A \\sim C52: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002
C48 \\sim C47 \\sim C46 \\sim C45: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
4. Others
 Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=
 Sof(H52D)=1-FVAR(1)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H50A)=Sof(H50B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C33(H33), C26(H26)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C46(H46A,H46B), C45(H45A,H45B), C49(H49A,H49B), C48(H48A,
 H48B), C47(H47A,H47B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B),
 C50(H50C,H50D), C51A(H51C,H51D), C52A(H52C,H52D)
5.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C1(H1), C29(H29), C31(H31), C13(H13), C2(H2), C22(H22), C30(H30),
 C4(H4), C3(H3), C10(H10), C19(H19), C16(H16), C14(H14), C20(H20), C7(H7),
 C15(H15), C21(H21), C9(H9), C8(H8)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C43(H43A,H43B,
 H43C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C28(H28A,H28B,H28C), C27(H27A,
 H27B,H27C)
;
_olex2_date_sample_data_collection 2021-10-23
_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 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.649