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_7712861
_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         'C86 H62 Br2 Ca2 N4 O4'
_chemical_formula_sum            'C86 H62 Br2 Ca2 N4 O4'
_chemical_formula_weight         1455.37
_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   geom
_atom_sites_solution_primary     dual
_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                78.371(2)
_cell_angle_beta                 70.616(3)
_cell_angle_gamma                68.461(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1141(4)
_cell_length_b                   12.0745(3)
_cell_length_c                   14.6995(5)
_cell_measurement_reflns_used    12175
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      71.6360
_cell_measurement_theta_min      4.4490
_cell_volume                     1723.71(11)
_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      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 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    -53.00  31.00   1.00    1.08    --  -35.97  57.00 -90.00   84
  2  \w   -103.00 -19.00   1.00    1.08    --  -35.97 -57.00 150.00   84
  3  \w    -53.00  31.00   1.00    1.08    --  -35.97  57.00 -30.00   84
  4  \w    -35.00  65.00   1.00    1.08    --   35.97 -19.00 -30.00  100
  5  \w     28.00  90.00   1.00    1.08    --   35.97-126.00-150.00   62
  6  \w     28.00  90.00   1.00    1.08    --   35.97-126.00 120.00   62
  7  \w     17.00 105.00   1.00    1.08    --   35.97  38.00 150.00   88
  8  \w      6.00  75.00   1.00    1.08    --   35.97 -99.00 -30.00   69
  9  \w     38.00 109.00   1.00    4.34    --  107.97-112.00 -30.00   71
 10  \w     40.00 125.00   1.00    4.34    --  107.97 -45.00-150.00   85
 11  \w    103.00 176.00   1.00    4.34    --  107.97  77.00-120.00   73
 12  \w     38.00 109.00   1.00    4.34    --  107.97-112.00 150.00   71
 13  \w     40.00 135.00   1.00    4.34    --  107.97 -77.00 150.00   95
 14  \w    101.00 176.00   1.00    4.34    --  107.97  84.00   8.00   75
 15  \w     38.00 109.00   1.00    4.34    --  107.97-112.00 120.00   71
 16  \w     38.00 129.00   1.00    4.34    --  107.97 -30.00 -60.00   91
 17  \w     40.00 135.00   1.00    4.34    --  107.97 -77.00 -30.00   95
 18  \w     38.00 109.00   1.00    4.34    --  107.97-112.00   0.00   71
 19  \w     38.00 109.00   1.00    4.34    --  107.97-112.00-120.00   71
 20  \w     40.00 125.00   1.00    4.34    --  107.97 -45.00  90.00   85
 21  \w     91.00 176.00   1.00    4.34    --  107.97  45.00  60.00   85
 22  \w     39.00 177.00   1.00    4.34    --  107.97   0.00-150.00  138
 23  \w     90.00 175.00   1.00    4.34    --  107.97  61.00 120.00   85
 24  \w     38.00 109.00   1.00    4.34    --  107.97-112.00  90.00   71
 25  \w   -103.00 -19.00   1.00    1.08    --  -35.97 -57.00 -30.00   84
 26  \w   -103.00 -19.00   1.00    1.08    --  -35.97 -57.00  30.00   84
 27  \w   -103.00 -19.00   1.00    1.08    --  -35.97 -57.00-120.00   84
 28  \w     19.00 103.00   1.00    1.08    --   35.97  57.00   0.00   84
 29  \w    -33.00  55.00   1.00    1.08    --   35.97 -38.00  90.00   88
;
_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      -0.0982969000
_diffrn_orient_matrix_UB_12      0.0265155000
_diffrn_orient_matrix_UB_13      -0.0608750000
_diffrn_orient_matrix_UB_21      -0.0791221000
_diffrn_orient_matrix_UB_22      -0.0743663000
_diffrn_orient_matrix_UB_23      0.0771676000
_diffrn_orient_matrix_UB_31      -0.0906572000
_diffrn_orient_matrix_UB_32      0.1128632000
_diffrn_orient_matrix_UB_33      0.0527784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19188
_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         71.789
_diffrn_reflns_theta_min         3.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73875
_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    1.402
_exptl_crystal_description       irregular
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0410P)^2^+0.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6135
_reflns_number_total             6652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        1723.70(10)
_cod_database_code               7712861
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 Ca1 O1 Br1 N1'
_reflns_odcompleteness_completeness 99.98
_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
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C17(H17), C10(H10), C34(H34), C35(H35), C37(H37), C8(H8), C36(H36),
 C4(H4), C18(H18), C20(H20), C40(H40), C32(H32), C42(H42), C7(H7), C5(H5),
 C19(H19), C41(H41), C6(H6), C13(H13), C31(H31), C23(H23), C11(H11), C29(H29),
 C26(H26), C30(H30), C12(H12), C24(H24), C25(H25)
;
_shelx_res_checksum              72981
_shelx_hkl_checksum              32608
_olex2_date_sample_data_collection 2022-10-13
_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 1.385
_oxdiff_exptl_absorpt_empirical_full_min 0.708