Synthesis, crystal structure and magnetic properties of the Re(ii) complexes NBu4[Re(NO)Br4(L)] (L = pyridine and diazine type ligands).
Pacheco, Mario; Cuevas, Alicia; González-Platas, Javier; Faccio, Ricardo; Lloret, Francesc; Julve, Miguel; Kremer, Carlos; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15361–15371; doi:10.1039/c3dt51699g

data_7023653
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of the Re(ii)
 complexes NBu4[Re(NO)Br4(L)] (L = pyridine and diazine type ligands).
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15361
_journal_page_last               15371
_journal_paper_doi               10.1039/c3dt51699g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C16 H36 N, C4 H4 Br4 N3 O Re'
_chemical_formula_sum            'C20 H40 Br4 N4 O Re'
_chemical_formula_weight         858.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-24
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.977(5)
_cell_angle_beta                 91.828(8)
_cell_angle_gamma                110.422(9)
_cell_formula_units_Z            2
_cell_length_a                   8.9061(12)
_cell_length_b                   10.8464(6)
_cell_length_c                   16.5056(11)
_cell_measurement_reflns_used    5993
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5280
_cell_measurement_theta_min      2.8725
_cell_volume                     1482.1(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0826849000
_diffrn_orient_matrix_UB_12      0.0082853000
_diffrn_orient_matrix_UB_13      0.0021428000
_diffrn_orient_matrix_UB_21      -0.0089797000
_diffrn_orient_matrix_UB_22      -0.0295659000
_diffrn_orient_matrix_UB_23      0.0367606000
_diffrn_orient_matrix_UB_31      -0.0185376000
_diffrn_orient_matrix_UB_32      -0.0632571000
_diffrn_orient_matrix_UB_33      -0.0228272000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13344
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.5280
_diffrn_reflns_theta_min         2.8725
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.4406
_exptl_crystal_size_mid          0.3312
_exptl_crystal_size_min          0.2706
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0133P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4489
_reflns_number_total             5214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51699g.txt
_cod_data_source_block           pyd
_cod_database_code               7023653
_reflns_odcompleteness_completeness 66.39
_reflns_odcompleteness_iscentric 0
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C31(H31A,H31B), C11(H11A,H11B), C41(H41A,H41B), C42(H42A,
 H42B), C22(H22A,H22B), C12(H12A,H12B), C32(H32A,H32B), C23(H23A,H23B),
 C33(H33A,H33B), C43(H43A,H43B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              21118
_shelxl_version_number           2012-9
_shelx_hkl_checksum              4113