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_7118305
_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            'C34 H47 B N6 O2 S3 Zn'
_chemical_formula_weight         744.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 119.4240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3568(8)
_cell_length_b                   19.5721(15)
_cell_length_c                   10.5278(11)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.18
_cell_measurement_theta_min      2.26
_cell_volume                     1858.8(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0576
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30599
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.974
_diffrn_reflns_theta_min         2.081
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11621
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0467
_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          0.0785
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.949
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.988
_reflns_number_gt                8983
_reflns_number_total             11621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08915h2.cif
_cod_data_source_block           pq
_cod_depositor_comments
'Adding full bibliography for 7118303--7118307.cif.'
_cod_database_code               7118305
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              75060