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_7712860
_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 Se'
_chemical_formula_sum            'C38 H49 Ca N5 Se'
_chemical_formula_weight         694.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5884(3)
_cell_length_b                   18.63906(18)
_cell_length_c                   19.03955(18)
_cell_measurement_reflns_used    8591
_cell_measurement_temperature    192(3)
_cell_measurement_theta_max      71.7240
_cell_measurement_theta_min      3.8480
_cell_volume                     8016.16(15)
_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      192(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_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   -103.00 -17.00   1.00    4.28    --  -36.22 -38.00 -90.00   86
  2  \w     33.00  84.00   1.00    4.28    --   36.22-126.00 -30.00   51
  3  \w     78.00 103.00   1.00    4.28    --   36.22   0.00-150.00   25
  4  \w    -17.00   9.00   1.00    4.28    --   36.22   0.00-150.00   26
  5  \w     42.00 105.00   1.00   17.13    --  107.97 -95.00-150.00   63
  6  \w    104.00 136.00   1.00   17.13    --  107.97  77.00-120.00   32
  7  \w    105.00 161.00   1.00   17.13    --  107.97  77.00 -30.00   56
  8  \w     96.00 175.00   1.00   17.13    --  107.97  45.00 120.00   79
  9  \w     57.00 126.00   1.00   17.13    --  107.97 -77.00   0.00   69
;
_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      -0.0012780000
_diffrn_orient_matrix_UB_12      0.0255285000
_diffrn_orient_matrix_UB_13      -0.0769580000
_diffrn_orient_matrix_UB_21      0.0675478000
_diffrn_orient_matrix_UB_22      0.0113129000
_diffrn_orient_matrix_UB_23      0.0019719000
_diffrn_orient_matrix_UB_31      0.0094180000
_diffrn_orient_matrix_UB_32      -0.0777589000
_diffrn_orient_matrix_UB_33      -0.0249689000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17326
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.882
_diffrn_reflns_theta_min         3.853
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78090
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0600P)^2^+4.9870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6549
_reflns_number_total             7694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        8016.14(14)
_cod_database_code               7712860
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 Ca1 Se1 '
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.624
_reflns_odcompleteness_completeness 99.76
_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. Uiso/Uaniso restraints and constraints
C2 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3: within 1.7A with sigma of
0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C36(H36), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C16(H16), C8(H8), C14(H14), C17(H17), C11(H11), C9(H9), C15(H15),
 C10(H10), C7(H7), C6(H6), C5(H5), C4(H4), C3(H3), C32(H32), C33(H33), C34(H34)
3.d Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
3.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C37(H37A,H37B,
 H37C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              60950
_shelx_hkl_checksum              89573
_shelx_fab_checksum              1189
_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 1.408
_oxdiff_exptl_absorpt_empirical_full_min 0.580