Alkylzinc-mediated transmetallation of a calcium hydride.
Pearce, Kyle G.; Mahon, Mary F.; Hill, Michael S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8903–8907; doi:10.1039/d5dt00958h

data_7718653
_publ_section_title
;
 Alkylzinc-mediated transmetallation of a calcium hydride.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8903
_journal_page_last               8907
_journal_paper_doi               10.1039/d5dt00958h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C73 H106 Ca2 N4, 2(C3.5 H4)'
_chemical_formula_sum            'C80 H114 Ca2 N4'
_chemical_formula_weight         1211.91
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2024-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-10 deposited with the CCDC.	2025-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.75490(10)
_cell_length_b                   21.8797(2)
_cell_length_c                   23.3417(2)
_cell_measurement_reflns_used    32026
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.2620
_cell_measurement_theta_min      4.3120
_cell_volume                     7486.65(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64762
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.379
_diffrn_reflns_theta_min         3.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         14829
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0771P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13354
_reflns_number_total             14829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00958h2.cif
_cod_data_source_block           s24msh20
_cod_depositor_comments
'Adding full bibliography for 7718652--7718654.cif.'
_cod_database_code               7718653
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-H30B = C30-H30A = C30-H30C
 0.98 with sigma of 0.005
 C85-C80 \\sim C85-C84 \\sim C85A-C80A \\sim C85A-C84A
 with sigma of 0.005
 C44A-C41 \\sim C44-C41 \\sim C42-C41 \\sim C42A-C41 \\sim C43-C41 \\sim
C43A-C41
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C79A \\sim C80A \\sim C81A \\sim C82A \\sim C83A \\sim C84A \\sim C85A \\sim
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C42 \\sim C43 \\sim C44 \\sim C42A \\sim C43A \\sim C44A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: H75(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) H43C(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C74(0.5) H74B(0.5)
 H74A(0.5) H74C(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C43A(0.5)
 H43D(0.5) H43E(0.5) H43F(0.5) C44A(0.5) H44D(0.5) H44E(0.5) H44F(0.5)
 C79A(0.33) C80A(0.33) H80A(0.33) C81A(0.33) H81A(0.33) C82A(0.33) H82A(0.33)
 C83A(0.33) H83A(0.33) C84A(0.33) H84A(0.33) C85A(0.33) H85D(0.33) H85E(0.33)
 H85F(0.33) C79(0.17) C80(0.17) H80(0.17) C81(0.17) H81(0.17) C82(0.17)
 H82(0.17) C83(0.17) H83(0.17) C84(0.17) H84(0.17) C85(0.17) H85B(0.17)
 H85A(0.17) H85C(0.17)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C56(H56), C59(H59), C68(H68), C71(H71)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C34(H34), C46(H46),
 C52(H52), C53(H53), C54(H54), C64(H64), C65(H65), C66(H66), C75(H75), C76(H76),
  C77(H77), C80A(H80A), C81A(H81A), C82A(H82A), C83A(H83A), C84A(H84A),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
5.c Fitted hexagon refined as free rotating group:
 C79A(C80A,C81A,C82A,C83A,C84A), C79(C80,C81,C82,C83,C84)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C74(H74B,H74A,H74C), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F), C44A(H44D,
 H44E,H44F), C85A(H85D,H85E,H85F), C85(H85B,H85A,H85C)
;
_shelx_res_checksum              84018
_shelx_hkl_checksum              90754
_olex2_submission_special_instructions 'No special instructions were received'