N-Heterocyclic carbene, carbodiphosphorane and diphosphine adducts of beryllium dihalides: synthesis, characterisation and reduction studies.
Paparo, Albert; Matthews, Aidan J. R.; Smith, Cory D.; Edwards, Alison J.; Yuvaraj, K.; Jones, Cameron; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7604–7609; doi:10.1039/d1dt01393a

data_7707383
_publ_section_title
;
 N-Heterocyclic carbene, carbodiphosphorane and diphosphine adducts of
 beryllium dihalides: synthesis, characterisation and reduction studies.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7604
_journal_page_last               7609
_journal_paper_doi               10.1039/d1dt01393a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_sum            'C37 H44 Be N2'
_chemical_formula_weight         525.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2007(4)
_cell_length_b                   14.1881(4)
_cell_length_c                   17.9562(5)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9680
_cell_measurement_theta_min      3.5220
_cell_volume                     3108.30(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.49a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19406
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 2095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                5253
_reflns_number_total             5749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01393a2.cif
_cod_data_source_block           Cj1486
_cod_depositor_comments
'Adding full bibliography for 7707372--7707383.cif.'
_cod_database_code               7707383
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              86730
_shelx_hkl_checksum              93709