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_7718654
_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         'C70 H112 Ca2 N4 Zn2, 2(C7 H8)'
_chemical_formula_sum            'C84 H128 Ca2 N4 Zn2'
_chemical_formula_weight         1404.80
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2024-08-09
_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                79.833(2)
_cell_angle_beta                 83.380(2)
_cell_angle_gamma                79.400(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3098(3)
_cell_length_b                   12.3970(2)
_cell_length_c                   14.7801(4)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.5790
_cell_measurement_theta_min      3.0470
_cell_volume                     1997.58(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23719
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.107
_diffrn_reflns_theta_min         3.049
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (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    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00058(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8418
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0553P)^2^+0.8063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7205
_reflns_number_total             8418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00958h2.cif
_cod_data_source_block           y24msh02
_cod_depositor_comments
'Adding full bibliography for 7718652--7718654.cif.'
_cod_database_code               7718654
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.581
_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
 C42-C37 \\sim C42-C41
 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
C36 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim C37 \\sim C42: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C30(H30), C33(H33)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C41(H41),
 C40(H40), C39(H39), C38(H38), C37(H37)
4.c Fitted hexagon refined as free rotating group:
 C36(C41,C40,C39,C38,C37)
4.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), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C42(H42C,H42B,H42A)
;
_shelx_res_checksum              98428
_shelx_hkl_checksum              28106
_olex2_submission_special_instructions 'No special instructions were received'