Synthesis and Group 4 Complexes of Tris(pyrrolyl-α-methyl)amine
Yanhui Shi; Changsheng Cao; Aaron L. Odom; Inorganic Chemistry 43 (2004) 275–281; doi:10.1021/ic035049v

data_4310352
_publ_section_title
;
 Synthesis and Group 4 Complexes of Tris(pyrrolyl-\a-methyl)amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              275
_journal_page_last               281
_journal_paper_doi               10.1021/ic035049v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C37 H49 Cl4 N7 Zr'
_chemical_formula_weight         824.85
_chemical_name_common            Zr(But-bpy)(NMe2)(tpa
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.270(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5527(18)
_cell_length_b                   23.370(5)
_cell_length_c                   20.101(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3965.2(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1419
_diffrn_reflns_av_sigmaI/netI    0.1525
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17955
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.583
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0043(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                3120
_reflns_number_total             5704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035049vsi20030908_104650_3.cif
_cod_data_source_block           shi501t
_cod_original_cell_volume        3965.1(14)
_cod_database_code               4310352