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_7712862
_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         'C60 H58 Br2 Ca2 N4 O4'
_chemical_formula_sum            'C60 H58 Br2 Ca2 N4 O4'
_chemical_formula_weight         1139.08
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2023-03-19 deposited with the CCDC.	2023-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2707(2)
_cell_length_b                   12.5295(2)
_cell_length_c                   17.6850(2)
_cell_measurement_reflns_used    7556
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      71.6760
_cell_measurement_theta_min      4.5860
_cell_volume                     2706.82(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(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 0.987
_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    -53.00  31.00   1.00    4.11    --  -35.97  57.00 -30.00   84
  2  \w    -88.00  -7.00   1.00    4.11    --  -35.97 126.00-150.00   81
  3  \w   -103.00 -19.00   1.00    4.11    --  -35.97 -57.00 120.00   84
  4  \w     28.00  90.00   1.00    4.11    --   35.97-126.00-150.00   62
  5  \w    -21.00  63.00   1.00    4.11    --   35.97 -77.00-180.00   84
  6  \w      6.00  75.00   1.00    4.11    --   35.97 -99.00  30.00   69
  7  \w     40.00 125.00   1.00   16.43    --  107.97 -45.00  90.00   85
  8  \w     40.00 135.00   1.00   16.43    --  107.97 -77.00   0.00   95
  9  \w     40.00 125.00   1.00   16.43    --  107.97 -45.00  30.00   85
 10  \w    103.00 176.00   1.00   16.43    --  107.97  77.00 120.00   73
 11  \w     39.00 106.00   1.00   16.43    --  107.97 -95.00   0.00   67
 12  \w     40.00 125.00   1.00   16.43    --  107.97 -45.00-180.00   85
 13  \w     39.00 106.00   1.00   16.43    --  107.97 -95.00-120.00   67
 14  \w     91.00 176.00   1.00   16.43    --  107.97  45.00  90.00   85
 15  \w    103.00 176.00   1.00   16.43    --  107.97  77.00-180.00   73
 16  \w   -103.00 -19.00   1.00    4.11    --  -35.97 -57.00 -60.00   84
;
_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      -0.1010817000
_diffrn_orient_matrix_UB_12      -0.0717788000
_diffrn_orient_matrix_UB_13      0.0045898000
_diffrn_orient_matrix_UB_21      0.0751872000
_diffrn_orient_matrix_UB_22      -0.0936328000
_diffrn_orient_matrix_UB_23      0.0271713000
_diffrn_orient_matrix_UB_31      -0.0063882000
_diffrn_orient_matrix_UB_32      0.0345446000
_diffrn_orient_matrix_UB_33      0.0830506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.763
_diffrn_reflns_theta_min         4.205
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33783
_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    1.398
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0600P)^2^+0.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4552
_reflns_number_total             5241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound7_CCDC1
_cod_database_code               7712862
_chemical_oxdiff_formula         'C1 H1 N1 Ca1 O1 Br1'
_reflns_odcompleteness_completeness 99.96
_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
2. Restrained distances
 C30-C29 \\sim C30-C29A \\sim C29A-C28 \\sim C29-C28 \\sim C28-C27
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C30 \\sim C29A \\sim C29 \\sim C28: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
4. Others
 Sof(H30C)=Sof(H30D)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C14(H14A,H14B), C30(H30A,H30B), C30(H30C,H30D), C28(H28A,
 H28B), C28(H28C,H28D), C29(H29A,H29B), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C12(H12), C3(H3), C15(H15), C26(H26), C11(H11), C23(H23), C4(H4),
 C20(H20), C18(H18), C6(H6), C5(H5), C24(H24), C9(H9), C10(H10), C25(H25),
 C19(H19)
;
_shelx_shelxl_version_number     2017/1
_olex2_date_sample_data_collection 2022-10-18
_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 2.247
_oxdiff_exptl_absorpt_empirical_full_min 0.672