#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:18:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179321 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321814.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_4321814
loop_
_publ_author_name
'Fred B. Stocker'
'Teodora P. Staeva'
'Chad M. Rienstra'
'Doyle Britton'
_publ_contact_author
;
Fred Stocker
Department of Chemistry
Macalester College
St. Paul, MN 55105
;
_publ_contact_author_email       stocker@macalester.edu
_publ_contact_author_fax         612-696-6432
_publ_contact_author_phone       612-696-6351
_publ_section_title
;
 Crystal Structures of a Series of Complexes Produced by Reaction of
 Copper(I) Cyanide with Diamines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              984
_journal_page_last               991
_journal_paper_doi               10.1021/ic970226b
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_sum            'C8 H16 Cu2 N4'
_chemical_formula_weight         295.34
_chemical_name_systematic
' N,N,N',N'-tetramethylethylenediamine/copper(I) cyanide complex'
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.889(4)
_cell_length_b                   33.380(8)
_cell_length_c                   9.012(3)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    297
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      10.0
_cell_volume                     3576.5(19)
_computing_cell_refinement       CAD-4
_computing_data_collection       CAD-4
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    TEXSAN
_diffrn_ambient_temperature      297
_diffrn_measurement_device       'CAD-4 diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K alpha'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5537
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         0
_diffrn_standards_decay_%        >1%
_diffrn_standards_interval_time  100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    35.50
_exptl_absorpt_correction_T_max  1.87
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.18
_refine_diff_density_min         -1.28
_refine_ls_abs_structure_details
;both polarities refined to the
      same wR value - one was chosen arbitrarily
;
_refine_ls_goodness_of_fit_obs   1.40
_refine_ls_hydrogen_treatment
'at idealized positions with B = 1.2 B of attached atom'
_refine_ls_matrix_type           full
_refine_ls_number_reflns         2983
_refine_ls_R_factor_obs          0.068
_refine_ls_shift/esd_max         0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(sigma squared F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.057
_reflns_number_observed          2983
_reflns_number_total             5534
_reflns_observed_criterion       'I > 2 sigma(I)'
_cod_data_source_file            ic970226b_7.cif
_cod_data_source_block           7-tetmen
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/(sigma squared F)' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/(sigma squared
F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3576(3)
_cod_database_code               4321814
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, z'
'x, -y, z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
CU1 0.5 0.53278(6) -0.1726 2.5(1)
CU2 0.5 0.64559(6) 0.1548(3) 2.9(1)
CU3 0.5 0.68148(6) -0.0640(3) 3.0(1)
CU4 0.5 0.79332(5) 0.2634(3) 2.90(9)
CU5 0.5 0.85757(5) 0.7612 2.91(9)
CU6 0.5 1.00536(5) 0.7515(3) 3.8(1)
C1N 0.5 0.4898(5) 0.133(2) 2.7(4)
N2C 0.5 0.5050(6) 0.022(2) 3.0(4)
C3N 0.5 0.6211(6) -0.066(2) 4.0(4)
N4C 0.5 0.5895(4) -0.120(1) 2.8(3)
C5N 0.5 0.7045(6) 0.160(2) 4.3(5)
N6C 0.5 0.7351(4) 0.215(1) 3.2(4)
N7C 0.5 0.8321(5) 0.569(2) 2.9(4)
C8N 0.5 0.8165(5) 0.449(2) 2.9(4)
C9N 0.5 0.8351(5) -0.051(2) 3.1(4)
N10C 0.5 0.8219(5) 0.072(1) 3.0(4)
N11C 0.5 0.9154(3) 0.755(2) 2.7(3)
C12N 0.5 0.9503(4) 0.749(2) 3.9(4)
N21 0.6222(8) 0.6174(3) 0.283(1) 3.3(5)
N31 0.6203(8) 0.7103(2) -0.1949(9) 2.8(5)
N61 0.6191(8) 1.0503(2) 0.756(1) 3.2(4)
C21 0.555(1) 0.6001(5) 0.406(2) 9(1)
C22 0.688(1) 0.5868(5) 0.208(2) 9(1)
C23 0.700(1) 0.6460(4) 0.347(2) 5.4(8)
C31 0.553(1) 0.7303(5) -0.301(2) 9(1)
C32 0.690(2) 0.7386(5) -0.108(2) 8(1)
C33 0.700(1) 0.6822(4) -0.260(2) 5.0(7)
C61 0.552(1) 1.0871(4) 0.764(3) 10(1)
C62 0.692(2) 1.0479(6) 0.881(2) 9(1)
C63 0.688(2) 1.0502(6) 0.622(2) 10(1)
H1 0.5774 0.6141 0.4934 10.4
H2 0.5774 0.5728 0.4140 10.4
H3 0.6382 0.5678 0.1640 10.5
H4 0.7351 0.5737 0.2771 10.5
H5 0.7321 0.5989 0.1324 10.5
H6 0.7433 0.6579 0.2699 6.5
H7 0.7485 0.6327 0.4143 6.5
H8 0.6590 0.6662 0.3978 6.5
H9 0.5742 0.7196 -0.3947 10.9
H10 0.5742 0.7577 -0.2961 10.9
H11 0.7418 0.7517 -0.1718 9.6
H12 0.7304 0.7242 -0.0338 9.6
H13 0.6430 0.7579 -0.0616 9.6
H14 0.6611 0.6631 -0.3186 6.0
H15 0.7404 0.6689 -0.1836 6.0
H16 0.7518 0.6965 -0.3213 6.0
H17 0.5744 1.1028 0.6818 12.3
H18 0.5744 1.1000 0.8536 12.3
H19 0.7349 1.0241 0.8756 10.3
H20 0.6485 1.0480 0.9695 10.3
H21 0.7410 1.0705 0.8812 10.3
H22 0.7302 1.0259 0.6179 11.5
H23 0.7386 1.0723 0.6247 11.5
H24 0.6413 1.0521 0.5375 11.5
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.000 0.000 'International Tables Vol IV Table 2.2A'
C C 0.002 0.002 'International Tables Vol IV Tables 2.2A and 2.3.1'
N N 0.004 0.003 'International Tables Vol IV Tables 2.2A and 2.3.1'
Cu Cu 0.263 1.266 'International Tables Vol IV Tables 2.2A and 2.3.1'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1N CU1 N2C 128.8(6)
C1N CU1 N4C 127.4(6)
N2C CU1 N4C 103.8(6)
CU3 CU2 C3N 53.6(5)
CU3 CU2 C5N 60.2(5)
CU3 CU2 N21 135.2(3)
C3N CU2 C5N 113.8(7)
C3N CU2 N21 110.0(4)
C5N CU2 N21 115.9(4)
N21 CU2 N21 88.5(5)
CU2 CU3 C3N 59.2(5)
CU2 CU3 C5N 52.1(5)
CU2 CU3 N31 136.2(2)
C3N CU3 C5N 111.3(7)
C3N CU3 N31 117.1(4)
C5N CU3 N31 111.4(4)
N31 CU3 N31 86.5(5)
N6C CU4 C8N 127.5(6)
N6C CU4 N10C 106.2(6)
C8N CU4 N10C 126.3(5)
N7C CU5 C9N 130.0(5)
N7C CU5 N11C 114.5(7)
C9N CU5 N11C 115.5(7)
C12N CU6 N61 136.7(3)
N61 CU6 N61 86.6(5)
CU1 C1N N2C 176(1)
CU1 N2C C1N 179(1)
CU2 C3N CU3 67.1(6)
CU2 C3N N4C 137(1)
CU3 C3N N4C 156(2)
CU1 N4C C3N 169(1)
CU2 C5N CU3 67.7(6)
CU2 C5N N6C 156(2)
CU3 C5N N6C 136(1)
CU4 N6C C5N 167(1)
CU5 N7C C8N 180(1)
CU4 C8N N7C 179(1)
CU5 C9N N10C 178(1)
CU4 N10C C9N 173(1)
CU5 N11C C12N 179(1)
CU6 C12N N11C 177(2)
CU2 N21 C21 102.6(8)
CU2 N21 C22 115.5(8)
CU2 N21 C23 111.6(8)
C21 N21 C22 111(1)
C21 N21 C23 107(1)
C22 N21 C23 108(1)
CU3 N31 C31 102.2(8)
CU3 N31 C32 112.2(7)
CU3 N31 C33 112.3(7)
C31 N31 C32 112(1)
C31 N31 C33 114(1)
C32 N31 C33 105(1)
CU6 N61 C61 103.9(8)
CU6 N61 C62 113.2(9)
CU6 N61 C63 111.6(9)
C61 N61 C62 110(1)
C61 N61 C63 110(1)
C62 N61 C63 108(1)
N21 C21 C21 122.4(7)
N21 C21 H1 106.25
N21 C21 H2 106.11
C21 C21 H1 106.13
C21 C21 H2 106.08
H1 C21 H2 109.50
N21 C22 H3 109.44
N21 C22 H4 109.45
N21 C22 H5 109.55
H3 C22 H4 109.38
H3 C22 H5 109.48
H4 C22 H5 109.53
N21 C23 H6 109.38
N21 C23 H7 109.42
N21 C23 H8 109.51
H6 C23 H7 109.41
H6 C23 H8 109.51
H7 C23 H8 109.60
N31 C31 C31 124.5(7)
N31 C31 H9 105.61
N31 C31 H10 105.63
C31 C31 H9 105.57
C31 C31 H10 105.58
H9 C31 H10 109.51
N31 C32 H11 109.50
N31 C32 H12 109.39
N31 C32 H13 109.53
H11 C32 H12 109.39
H11 C32 H13 109.58
H12 C32 H13 109.44
N31 C33 H14 109.46
N31 C33 H15 109.48
N31 C33 H16 109.44
H14 C33 H15 109.52
H14 C33 H16 109.45
H15 C33 H16 109.49
N61 C61 C61 122.8(7)
N61 C61 H17 106.15
N61 C61 H18 105.99
C61 C61 H17 106.00
C61 C61 H18 105.93
H17 C61 H18 109.62
N61 C62 H19 109.67
N61 C62 H20 109.44
N61 C62 H21 109.44
H19 C62 H20 109.52
H19 C62 H21 109.54
H20 C62 H21 109.21
N61 C63 H22 109.44
N61 C63 H23 109.51
N61 C63 H24 109.35
H22 C63 H23 109.61
H22 C63 H24 109.42
H23 C63 H24 109.51
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
CU1 C1N 1.90(2) 66403
CU1 N2C 1.98(2) 1
CU1 N4C 1.95(1) 1
CU2 CU3 2.307(2) 1
CU2 C3N 2.15(2) 1
CU2 C5N 1.97(2) 1
CU2 N21 2.08(1) 1
CU3 C3N 2.02(2) 1
CU3 C5N 2.16(2) 1
CU3 N31 2.087(9) 1
CU4 N6C 1.99(1) 1
CU4 C8N 1.84(2) 1
CU4 N10C 1.97(1) 1
CU5 N7C 1.93(2) 1
CU5 C9N 1.85(2) 55601
CU5 N11C 1.93(1) 1
CU6 C12N 1.84(1) 1
CU6 N61 2.063(8) 1
C1N N2C 1.13(2) 1
C3N N4C 1.16(2) 1
C5N N6C 1.13(2) 1
N7C C8N 1.20(2) 1
C9N N10C 1.19(2) 1
N11C C12N 1.17(1) 1
N21 C21 1.48(2) 1
N21 C22 1.45(1) 1
N21 C23 1.45(1) 1
N31 C31 1.42(1) 1
N31 C32 1.48(2) 1
N31 C33 1.46(1) 1
N61 C61 1.46(1) 1
N61 C62 1.42(2) 1
N61 C63 1.46(2) 1
C21 C21 1.31(3) 65502
C21 H1 0.948 1
C21 H2 0.951 1
C22 H3 0.951 1
C22 H4 0.950 1
C22 H5 0.949 1
C23 H6 0.951 1
C23 H7 0.950 1
C23 H8 0.949 1
C31 C31 1.25(3) 65502
C31 H9 0.950 1
C31 H10 0.949 1
C32 H11 0.950 1
C32 H12 0.951 1
C32 H13 0.949 1
C33 H14 0.950 1
C33 H15 0.950 1
C33 H16 0.950 1
C61 C61 1.25(3) 65502
C61 H17 0.947 1
C61 H18 0.951 1
C62 H19 0.948 1
C62 H20 0.952 1
C62 H21 0.951 1
C63 H22 0.950 1
C63 H23 0.949 1
C63 H24 0.9511 1
