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_7712863
_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         'C31 H42 Ca I N5'
_chemical_formula_sum            'C31 H42 Ca I N5'
_chemical_formula_weight         651.67
_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             2022-08-26
_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                89.334(3)
_cell_angle_beta                 74.032(3)
_cell_angle_gamma                70.382(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9398(3)
_cell_length_b                   10.1072(4)
_cell_length_c                   17.2990(6)
_cell_measurement_reflns_used    14036
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.1230
_cell_measurement_theta_min      3.8600
_cell_volume                     1567.60(10)
_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      180.00(10)
_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 0.887
_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    -10.00  84.00   1.00    6.07    --   16.35  77.00  60.00   94
  2  \w    -51.00  43.00   1.00    6.07    --   16.35 -77.00 -60.00   94
  3  \w    -51.00  33.00   1.00    6.07    --   16.35 -57.00-180.00   84
  4  \w    -10.00  84.00   1.00    6.07    --   16.35  77.00 -90.00   94
  5  \w    -33.00  51.00   1.00    6.07    --  -16.50  57.00 -30.00   84
  6  \w    -43.00  51.00   1.00    6.07    --  -16.50  77.00 150.00   94
  7  \w     35.00  89.00   1.00    6.07    --   16.35 178.00 150.00   54
  8  \w    -20.00  55.00   1.00    6.07    --   16.35 -99.00  60.00   75
  9  \w     -3.00  45.00   1.00    6.07    --   16.35  38.00  30.00   48
 10  \w    -84.00   0.00   1.00    6.07    --  -16.50 -57.00 150.00   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      -0.0753221000
_diffrn_orient_matrix_UB_12      0.0381998000
_diffrn_orient_matrix_UB_13      0.0213553000
_diffrn_orient_matrix_UB_21      0.0120603000
_diffrn_orient_matrix_UB_22      -0.0299944000
_diffrn_orient_matrix_UB_23      0.0358540000
_diffrn_orient_matrix_UB_31      0.0209547000
_diffrn_orient_matrix_UB_32      0.0568882000
_diffrn_orient_matrix_UB_33      0.0095843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27744
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.298
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92066
_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            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0120P)^2^+2.5480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6762
_reflns_number_total             7607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00301a2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        1567.60(9)
_cod_database_code               7712863
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 Ca1 I1 O1'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C1(H1), C2(H2), C10(H10), C18(H18), C17(H17), C9(H9), C16(H16),
 C4(H4), C3(H3), C8(H8), C7(H7)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,
 H31B,H31C)
;
_olex2_date_sample_data_collection 2021-11-16
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.855