Synthesis, structure and reactivity of [Tm(Bu(t))]ZnH, a monomeric terminal zinc hydride compound in a sulfur-rich coordination environment: access to a heterobimetallic compound.
Kreider-Mueller, Ava; Quinlivan, Patrick J.; Rauch, Michael; Owen, Jonathan S.; Parkin, Gerard; Chemical communications (Cambridge, England) 52 (2016) 2358–2361; doi:10.1039/c5cc08915h

data_7118303
_publ_section_title
;
 Synthesis, structure and reactivity of [Tm(Bu(t))]ZnH, a monomeric
 terminal zinc hydride compound in a sulfur-rich coordination environment:
 access to a heterobimetallic compound.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2358
_journal_page_last               2361
_journal_paper_doi               10.1039/c5cc08915h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C24 H38 B N6 S3 Zn'
_chemical_formula_weight         582.96
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-20 deposited with the CCDC.
2015-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.3984(11)
_cell_length_b                   13.3984(11)
_cell_length_c                   27.542(2)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.94
_cell_measurement_theta_min      2.22
_cell_volume                     4281.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            22244
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.771
_diffrn_reflns_theta_min         1.904
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1842
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2288
_reflns_number_total             3358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08915h2.cif
_cod_data_source_block           tmhs10pq
_cod_depositor_comments
;
Adding full bibliography for 7118303--7118307.cif.

2018-09-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H76 B2 N12 S6 Zn2'
_cod_original_formula_weight         1165.92
_cod_original_formula_units_Z            3
_cod_original_cell_volume        4281.9(8)
_cod_database_code               7118303
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.818
_shelx_res_checksum              74383