Group-4 η1-Pyrrolyl Complexes Incorporating N,N-Di(pyrrolyl-α-methyl)-N-methylamine
Yahong Li; Angie Turnas; James T. Ciszewski; Aaron L. Odom; Inorganic Chemistry 41 (2002) 6298–6306; doi:10.1021/ic0259484

data_4318969
_publ_section_title
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 Group-4 \h1-Pyrrolyl Complexes Incorporating
 N,N-Di(pyrrolyl-\a-methyl)-N-methylamine
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6298
_journal_page_last               6306
_journal_paper_doi               10.1021/ic0259484
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C23 H28 Cl2 Hf N6'
_chemical_formula_weight         637.90
_chemical_name_common            Hf(dpma)2.CH2Cl2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.97(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.47(2)
_cell_length_b                   17.56(5)
_cell_length_c                   15.95(4)
_cell_measurement_temperature    417(2)
_cell_volume                     2367(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      417(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1430
_diffrn_reflns_av_sigmaI/netI    0.1107
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10192
_diffrn_reflns_theta_full        23.55
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.4984
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.43
_refine_diff_density_max         3.511
_refine_diff_density_min         -3.467
_refine_diff_density_rms         0.412
_refine_ls_extinction_coef       0.0016(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   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                2814
_reflns_number_total             3465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259484_4.cif
_cod_data_source_block           yahong3f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2368(11)
_cod_database_code               4318969