#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:35:12 +0100 (vie 25 de mar de 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009337.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009337
loop_
_publ_author_name
'He, Zhicong'
'Chaimungkalanont, P. Jinny'
'Craig, Donald C.'
'Colbran, Stephen B.'
_publ_section_title
;
 Copper(II) complexes of 6-hydroxymethyl-substituted
 tris(2-pyridylmethyl)amine ligands †
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1419
_journal_paper_doi               10.1039/b000092m
_journal_year                    2000
_chemical_formula_moiety
'C21 H24 Br0.43 Cl0.57 Cu N4 O3 1+,0.5(Br2.8 Cl1.2 Cu 2-)'
_chemical_formula_sum            'C21 H24 Br1.83 Cl1.18 Cu1.5 N4 O3'
_chemical_formula_weight         663.0
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                90
_cell_angle_beta                 90.77(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.310(4)
_cell_length_b                   10.311(1)
_cell_length_c                   28.039(6)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      20
_cell_measurement_theta_min      18
_cell_volume                     4715.0(16)
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_number            3577
_diffrn_reflns_theta_max         60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    6.934
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_density_diffrn    1.87
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2634.1
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.36
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     297
_refine_ls_number_reflns         2291
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0016F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                2291
_reflns_number_total             3497
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            b000092m.txt
_cod_data_source_block           COMPOUND5
_cod_original_cell_volume        4715(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7009337
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t-min  0.53
_exptl_absorpt_correction_t-max  0.82
_diffrn_reflns_h_min             -18
_diffrn_reflns_h_max             18
_diffrn_reflns_k_min             0
_diffrn_reflns_k_max             11
_diffrn_reflns_l_min             0
_diffrn_reflns_l_max             31
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,-y,1/2+z
3 -x,-y,-z
4 -x,y,1/2-z
5 1/2+x,1/2+y,z
6 1/2+x,1/2-y,1/2+z
7 1/2-x,1/2-y,-z
8 1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_type_symbol
_atom_site_occupancy
Cu1 0.24821(4) 0.47280(6) 0.08095(2) 0.0390(2) Uani Cu ?
Br/Cl1 0.21815(5) 0.56154(8) 0.00694(3) 0.0495(3) Uani Br/Cl1 ?
O1 0.1860(2) 0.3004(3) 0.0693(1) 0.0375(8) Uani O ?
O2 0.0405(2) 0.4007(3) 0.0815(1) 0.0452(8) Uani O ?
O3 0.4401(2) 0.0843(3) 0.0315(1) 0.056(1) Uani O ?
N1 0.2732(2) 0.3848(3) 0.1398(1) 0.0321(9) Uani N ?
N2 0.1456(2) 0.5985(3) 0.1227(1) 0.0383(9) Uani N ?
N3 0.3983(2) 0.4179(4) 0.0653(1) 0.0386(9) Uani N ?
N4 0.3148(2) 0.6236(4) 0.1106(1) 0.0386(9) Uani N ?
C1 0.3387(3) 0.5862(5) 0.1606(2) 0.044(1) Uani C ?
C2 0.3198(3) 0.4472(5) 0.1722(2) 0.036(1) Uani C ?
C3 0.3470(3) 0.3845(5) 0.2131(2) 0.046(1) Uani C ?
C4 0.3249(3) 0.2557(5) 0.2193(2) 0.050(1) Uani C ?
C5 0.2773(3) 0.1925(5) 0.1856(2) 0.045(1) Uani C ?
C6 0.2518(3) 0.2620(4) 0.1459(2) 0.035(1) Uani C ?
C7 0.1988(3) 0.2072(5) 0.1063(2) 0.040(1) Uani C ?
C8 0.2627(3) 0.7425(4) 0.1109(2) 0.044(1) Uani C ?
C9 0.1784(3) 0.7162(4) 0.1315(2) 0.038(1) Uani C ?
C10 0.1374(3) 0.8123(5) 0.1561(2) 0.044(1) Uani C ?
C11 0.0587(3) 0.7878(5) 0.1718(2) 0.049(1) Uani C ?
C12 0.0251(3) 0.6667(5) 0.1628(2) 0.046(1) Uani C ?
C13 0.0696(3) 0.5753(4) 0.1386(2) 0.038(1) Uani C ?
C14 0.0353(3) 0.4431(5) 0.1299(2) 0.049(1) Uani C ?
C15 0.3875(3) 0.6509(5) 0.0808(2) 0.044(1) Uani C ?
C16 0.4379(3) 0.5315(5) 0.0702(2) 0.042(1) Uani C ?
C17 0.5213(3) 0.5444(5) 0.0624(2) 0.043(1) Uani C ?
C18 0.5649(3) 0.4360(6) 0.0493(2) 0.049(1) Uani C ?
C19 0.5256(3) 0.3180(5) 0.0446(2) 0.044(1) Uani C ?
C20 0.4421(3) 0.3139(5) 0.0530(2) 0.036(1) Uani C ?
C21 0.3937(3) 0.1902(5) 0.0509(2) 0.048(1) Uani C ?
Cu2 0.00000 0.27027(9) 0.25000 0.0391(3) Uani Cu ?
Br/Cl2 0.11328(4) 0.41109(6) 0.26244(2) 0.0629(3) Uani Br/Cl2 ?
Br/Cl3 0.05824(5) 0.12279(7) 0.19811(3) 0.0469(3) Uani Br/Cl3 ?
HO1 0.1285 0.3335 0.0672 0.038 Uani H ?
HO2 0.0173 0.4722 0.0613 0.045 Uani H ?
HO3 0.3952 0.0184 0.0322 0.056 Uani H ?
H1C1 0.3084 0.6431 0.1833 0.044 Uani H ?
H2C1 0.3990 0.6003 0.1649 0.044 Uani H ?
HC3 0.3815 0.4307 0.2375 0.046 Uani H ?
HC4 0.3436 0.2082 0.2486 0.050 Uani H ?
HC5 0.2618 0.0994 0.1897 0.045 Uani H ?
H1C7 0.1446 0.1815 0.1196 0.040 Uani H ?
H2C7 0.2264 0.1291 0.0927 0.040 Uani H ?
H1C8 0.2556 0.7743 0.0774 0.044 Uani H ?
H2C8 0.2907 0.8106 0.1305 0.044 Uani H ?
HC10 0.1641 0.8981 0.1623 0.044 Uani H ?
HC11 0.0271 0.8555 0.1893 0.049 Uani H ?
HC12 -0.0315 0.6459 0.1737 0.046 Uani H ?
H1C14 -0.0238 0.4435 0.1391 0.049 Uani H ?
H2C14 0.0661 0.3801 0.1505 0.049 Uani H ?
H1C15 0.4232 0.7148 0.0981 0.044 Uani H ?
H2C15 0.3681 0.6892 0.0499 0.044 Uani H ?
HC17 0.5490 0.6303 0.0661 0.043 Uani H ?
HC18 0.6250 0.4428 0.0433 0.049 Uani H ?
HC19 0.5564 0.2381 0.0354 0.044 Uani H ?
H1C21 0.3439 0.2043 0.0304 0.048 Uani H ?
H2C21 0.3767 0.1668 0.0839 0.048 Uani H ?
loop_
_atom_type_symbol
_atom_type_description
Br/Cl1 0.43Br+0.57Cl
Br/Cl2 0.97Br+0.03Cl
Br/Cl3 0.43Br+0.57Cl
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br/Cl1 Cu1 O1 95.8(1) 1_555 1_555 1_555 no
Br/Cl1 Cu1 N1 175.1(1) 1_555 1_555 1_555 no
Br/Cl1 Cu1 N2 94.7(1) 1_555 1_555 1_555 no
Br/Cl1 Cu1 N3 97.2(1) 1_555 1_555 1_555 no
Br/Cl1 Cu1 N4 99.6(1) 1_555 1_555 1_555 no
O1 Cu1 N1 80.1(1) 1_555 1_555 1_555 no
O1 Cu1 N2 101.2(1) 1_555 1_555 1_555 no
O1 Cu1 N3 104.5(1) 1_555 1_555 1_555 no
O1 Cu1 N4 164.5(1) 1_555 1_555 1_555 no
N1 Cu1 N2 88.8(1) 1_555 1_555 1_555 no
N1 Cu1 N3 81.4(1) 1_555 1_555 1_555 no
N1 Cu1 N4 84.6(1) 1_555 1_555 1_555 no
N2 Cu1 N3 150.2(1) 1_555 1_555 1_555 no
N2 Cu1 N4 76.5(1) 1_555 1_555 1_555 no
N3 Cu1 N4 74.7(1) 1_555 1_555 1_555 no
Cu1 O1 C7 113.4(2) 1_555 1_555 1_555 no
Cu1 N1 C2 117.8(3) 1_555 1_555 1_555 no
Cu1 N1 C6 120.6(3) 1_555 1_555 1_555 no
C2 N1 C6 121.2(4) 1_555 1_555 1_555 no
Cu1 N2 C9 107.1(3) 1_555 1_555 1_555 no
Cu1 N2 C13 135.1(3) 1_555 1_555 1_555 no
C9 N2 C13 117.7(4) 1_555 1_555 1_555 no
Cu1 N3 C16 104.5(3) 1_555 1_555 1_555 no
Cu1 N3 C20 137.7(3) 1_555 1_555 1_555 no
C16 N3 C20 117.8(4) 1_555 1_555 1_555 no
Cu1 N4 C1 108.1(3) 1_555 1_555 1_555 no
Cu1 N4 C8 108.9(3) 1_555 1_555 1_555 no
Cu1 N4 C15 109.6(3) 1_555 1_555 1_555 no
C1 N4 C8 110.3(4) 1_555 1_555 1_555 no
C1 N4 C15 112.0(3) 1_555 1_555 1_555 no
C8 N4 C15 107.9(4) 1_555 1_555 1_555 no
N4 C1 C2 113.3(4) 1_555 1_555 1_555 no
N1 C2 C1 115.3(4) 1_555 1_555 1_555 no
N1 C2 C3 120.7(4) 1_555 1_555 1_555 no
C1 C2 C3 124.0(4) 1_555 1_555 1_555 no
C2 C3 C4 118.0(4) 1_555 1_555 1_555 no
C3 C4 C5 120.8(5) 1_555 1_555 1_555 no
C4 C5 C6 117.9(4) 1_555 1_555 1_555 no
N1 C6 C5 121.5(4) 1_555 1_555 1_555 no
N1 C6 C7 114.3(4) 1_555 1_555 1_555 no
C5 C6 C7 124.2(4) 1_555 1_555 1_555 no
O1 C7 C6 111.1(4) 1_555 1_555 1_555 no
N4 C8 C9 111.9(4) 1_555 1_555 1_555 no
N2 C9 C8 116.7(4) 1_555 1_555 1_555 no
N2 C9 C10 122.9(4) 1_555 1_555 1_555 no
C8 C9 C10 120.4(4) 1_555 1_555 1_555 no
C9 C10 C11 118.9(4) 1_555 1_555 1_555 no
C10 C11 C12 118.1(4) 1_555 1_555 1_555 no
C11 C12 C13 119.9(5) 1_555 1_555 1_555 no
N2 C13 C12 122.5(4) 1_555 1_555 1_555 no
N2 C13 C14 117.0(4) 1_555 1_555 1_555 no
C12 C13 C14 120.5(4) 1_555 1_555 1_555 no
O2 C14 C13 114.0(4) 1_555 1_555 1_555 no
N4 C15 C16 113.4(4) 1_555 1_555 1_555 no
N3 C16 C15 117.9(4) 1_555 1_555 1_555 no
N3 C16 C17 122.6(5) 1_555 1_555 1_555 no
C15 C16 C17 119.4(4) 1_555 1_555 1_555 no
C16 C17 C18 118.4(4) 1_555 1_555 1_555 no
C17 C18 C19 120.1(4) 1_555 1_555 1_555 no
C18 C19 C20 117.7(5) 1_555 1_555 1_555 no
N3 C20 C19 123.4(4) 1_555 1_555 1_555 no
N3 C20 C21 114.2(4) 1_555 1_555 1_555 no
C19 C20 C21 122.4(4) 1_555 1_555 1_555 no
O3 C21 C20 112.4(4) 1_555 1_555 1_555 no
Br/Cl2 Cu2 Br/Cl3 99.7(1) 1_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Br/Cl1 2.314(1) 1_555 1_555 no
Cu1 O1 2.070(3) 1_555 1_555 no
Cu1 N1 1.921(4) 1_555 1_555 no
Cu1 N2 2.429(4) 1_555 1_555 no
Cu1 N3 2.556(4) 1_555 1_555 no
Cu1 N4 2.066(4) 1_555 1_555 no
O1 C7 1.427(5) 1_555 1_555 no
O2 C14 1.430(6) 1_555 1_555 no
O3 C21 1.438(6) 1_555 1_555 no
N1 C2 1.340(5) 1_555 1_555 no
N1 C6 1.326(5) 1_555 1_555 no
N2 C9 1.347(5) 1_555 1_555 no
N2 C13 1.345(6) 1_555 1_555 no
N3 C16 1.344(6) 1_555 1_555 no
N3 C20 1.336(6) 1_555 1_555 no
N4 C1 1.501(6) 1_555 1_555 no
N4 C8 1.492(6) 1_555 1_555 no
N4 C15 1.485(6) 1_555 1_555 no
C1 C2 1.502(6) 1_555 1_555 no
C2 C3 1.385(6) 1_555 1_555 no
C3 C4 1.388(7) 1_555 1_555 no
C4 C5 1.378(7) 1_555 1_555 no
C5 C6 1.383(6) 1_555 1_555 no
C6 C7 1.507(6) 1_555 1_555 no
C8 C9 1.523(6) 1_555 1_555 no
C9 C10 1.385(6) 1_555 1_555 no
C10 C11 1.387(6) 1_555 1_555 no
C11 C12 1.386(7) 1_555 1_555 no
C12 C13 1.374(6) 1_555 1_555 no
C13 C14 1.493(6) 1_555 1_555 no
C15 C16 1.512(6) 1_555 1_555 no
C16 C17 1.386(6) 1_555 1_555 no
C17 C18 1.377(7) 1_555 1_555 no
C18 C19 1.380(7) 1_555 1_555 no
C19 C20 1.387(6) 1_555 1_555 no
C20 C21 1.501(6) 1_555 1_555 no
Cu2 Br/Cl2 2.372(1) 1_555 1_555 no
Cu2 Br/Cl3 2.317(1) 1_555 1_555 no
