#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:20:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178504 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/60/4066010.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_4066010
loop_
_publ_author_name
'Ma, Guibin'
'Ferguson, Michael J.'
'McDonald, Robert'
'Cavell, Ronald G.'
_publ_section_title
;
 Rare, Hexatomic, Boat-Shaped, Cross-Linked
 Bis(iminodiphenylphosphorano)methanediide Pincer Carbon Bridged
 Photoluminescent Copper Clusters Capped with Methyl or Halide Bridges
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4251
_journal_paper_doi               10.1021/om1002478
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C35 H50 Cu I N2 O P2 Si2'
_chemical_formula_sum            'C35 H50 Cu I N2 O P2 Si2'
_chemical_formula_weight         823.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 109.6397(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4818(4)
_cell_length_b                   18.8992(7)
_cell_length_c                   11.7168(4)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.28
_cell_volume                     1977.49(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω 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  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13831
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.7257
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0463P)²+2.2873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                4232
_reflns_number_total             4678
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om1002478_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4066010
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I I 0.17031(2) 0.2500 0.50424(3) 0.04597(10) Uani 1 2 d S
Cu Cu 0.43814(5) 0.2500 0.64125(4) 0.03089(11) Uani 1 2 d S
P P 0.71169(6) 0.16708(3) 0.65822(5) 0.02066(12) Uani 1 1 d .
Si Si 0.48694(7) 0.09884(3) 0.75832(6) 0.02801(14) Uani 1 1 d .
N N 0.5742(2) 0.16428(10) 0.70418(17) 0.0246(4) Uani 1 1 d .
C10 C 0.8149(3) 0.2500 0.6996(3) 0.0228(6) Uani 1 2 d S
H10A H 0.8947 0.2500 0.6626 0.027 Uiso 1 2 calc SR
H10B H 0.8651 0.2500 0.7886 0.027 Uiso 1 2 calc SR
C11 C 0.8507(2) 0.09896(12) 0.7209(2) 0.0253(4) Uani 1 1 d .
C12 C 0.9525(3) 0.10488(13) 0.8388(2) 0.0289(5) Uani 1 1 d .
H12 H 0.9555 0.1468 0.8843 0.035 Uiso 1 1 calc R
C13 C 1.0489(3) 0.04956(15) 0.8893(2) 0.0360(5) Uani 1 1 d .
H13 H 1.1186 0.0539 0.9691 0.043 Uiso 1 1 calc R
C14 C 1.0443(4) -0.01168(16) 0.8246(3) 0.0486(7) Uani 1 1 d .
H14 H 1.1104 -0.0496 0.8601 0.058 Uiso 1 1 calc R
C15 C 0.9441(4) -0.01827(17) 0.7081(3) 0.0567(9) Uani 1 1 d .
H15 H 0.9410 -0.0606 0.6637 0.068 Uiso 1 1 calc R
C16 C 0.8477(3) 0.03727(14) 0.6563(2) 0.0423(6) Uani 1 1 d .
H16 H 0.7794 0.0329 0.5760 0.051 Uiso 1 1 calc R
C17 C 0.3605(3) 0.04526(15) 0.6323(3) 0.0434(7) Uani 1 1 d .
H17A H 0.2892 0.0765 0.5742 0.052 Uiso 1 1 calc R
H17B H 0.3057 0.0112 0.6648 0.052 Uiso 1 1 calc R
H17C H 0.4199 0.0197 0.5914 0.052 Uiso 1 1 calc R
C18 C 0.3743(3) 0.14238(18) 0.8408(3) 0.0469(7) Uani 1 1 d .
H18A H 0.3013 0.1744 0.7857 0.056 Uiso 1 1 calc R
H18B H 0.4406 0.1695 0.9092 0.056 Uiso 1 1 calc R
H18C H 0.3215 0.1063 0.8710 0.056 Uiso 1 1 calc R
C19 C 0.6228(3) 0.03791(16) 0.8680(3) 0.0440(7) Uani 1 1 d .
H19A H 0.6898 0.0656 0.9352 0.053 Uiso 1 1 calc R
H19B H 0.6819 0.0128 0.8265 0.053 Uiso 1 1 calc R
H19C H 0.5676 0.0036 0.8995 0.053 Uiso 1 1 calc R
C21 C 0.6628(2) 0.15844(12) 0.49618(19) 0.0237(4) Uani 1 1 d .
C22 C 0.5135(3) 0.14867(13) 0.4250(2) 0.0303(5) Uani 1 1 d .
H22 H 0.4381 0.1479 0.4617 0.036 Uiso 1 1 calc R
C23 C 0.4746(3) 0.14010(15) 0.3003(2) 0.0406(6) Uani 1 1 d .
H23 H 0.3727 0.1333 0.2519 0.049 Uiso 1 1 calc R
C24 C 0.5837(4) 0.14148(15) 0.2469(2) 0.0428(7) Uani 1 1 d .
H24 H 0.5567 0.1357 0.1617 0.051 Uiso 1 1 calc R
C25 C 0.7322(4) 0.15116(14) 0.3167(2) 0.0398(6) Uani 1 1 d .
H25 H 0.8067 0.1521 0.2791 0.048 Uiso 1 1 calc R
C26 C 0.7728(3) 0.15954(13) 0.4412(2) 0.0318(5) Uani 1 1 d .
H26 H 0.8750 0.1660 0.4890 0.038 Uiso 1 1 calc R
O1S O -0.0164(3) 0.2500 0.0347(2) 0.0358(6) Uani 1 2 d S
C1S C 0.1323(6) 0.2500 0.1002(4) 0.097(3) Uani 1 2 d S
H1SA H 0.1533 0.2078 0.1535 0.117 Uiso 0.50 1 calc PR
H1SB H 0.1533 0.2922 0.1535 0.117 Uiso 0.50 1 calc PR
C2S C 0.2335(5) 0.2500 0.0369(4) 0.0624(14) Uani 1 2 d S
H2SA H 0.3360 0.2500 0.0946 0.075 Uiso 1 2 calc SR
H2SB H 0.2178 0.2923 -0.0141 0.075 Uiso 0.50 1 calc PR
H2SC H 0.2178 0.2077 -0.0141 0.075 Uiso 0.50 1 calc PR
C3S C -0.1201(6) 0.2500 0.0927(5) 0.096(3) Uani 1 2 d S
H3SA H -0.1007 0.2921 0.1460 0.115 Uiso 0.50 1 calc PR
H3SB H -0.1007 0.2079 0.1460 0.115 Uiso 0.50 1 calc PR
C4S C -0.2704(5) 0.2500 0.0246(4) 0.0711(18) Uani 1 2 d S
H4SA H -0.3298 0.2500 0.0788 0.085 Uiso 1 2 calc SR
H4SB H -0.2940 0.2077 -0.0266 0.085 Uiso 0.50 1 calc PR
H4SC H -0.2940 0.2923 -0.0266 0.085 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
N Cu N 104.57(11) 4_565 .
N Cu I 127.64(5) 4_565 .
N Cu I 127.64(5) . .
N P C21 114.12(10) . .
N P C11 114.33(10) . .
C21 P C11 104.88(10) . .
N P C10 111.78(12) . .
C21 P C10 106.40(12) . .
C11 P C10 104.49(11) . .
N Si C18 107.77(12) . .
N Si C17 111.10(12) . .
C18 Si C17 108.94(15) . .
N Si C19 112.84(11) . .
C18 Si C19 107.35(15) . .
C17 Si C19 108.71(14) . .
P N Si 135.03(12) . .
P N Cu 110.20(10) . .
Si N Cu 112.19(10) . .
P C10 P 118.36(16) . 4_565
C16 C11 C12 119.2(2) . .
C16 C11 P 119.87(18) . .
C12 C11 P 120.65(18) . .
C13 C12 C11 119.9(2) . .
C14 C13 C12 120.4(2) . .
C13 C14 C15 120.2(2) . .
C14 C15 C16 119.8(3) . .
C11 C16 C15 120.5(2) . .
C22 C21 C26 119.5(2) . .
C22 C21 P 119.49(17) . .
C26 C21 P 121.04(17) . .
C23 C22 C21 120.1(2) . .
C24 C23 C22 120.0(3) . .
C23 C24 C25 120.4(2) . .
C24 C25 C26 120.3(3) . .
C25 C26 C21 119.7(2) . .
C1S O1S C3S 120.1(4) . .
O1S C1S C2S 117.9(4) . .
O1S C3S C4S 119.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I Cu 2.5071(5) .
Cu N 2.0480(19) 4_565
Cu N 2.0480(19) .
P N 1.5694(19) .
P C21 1.804(2) .
P C11 1.812(2) .
P C10 1.8249(16) .
Si N 1.7235(19) .
Si C18 1.856(3) .
Si C17 1.858(3) .
Si C19 1.877(3) .
C10 P 1.8249(16) 4_565
C11 C16 1.385(3) .
C11 C12 1.399(3) .
C12 C13 1.383(3) .
C13 C14 1.376(4) .
C14 C15 1.381(4) .
C15 C16 1.390(4) .
C21 C22 1.393(3) .
C21 C26 1.398(3) .
C22 C23 1.391(3) .
C23 C24 1.377(4) .
C24 C25 1.382(4) .
C25 C26 1.387(4) .
O1S C1S 1.361(5) .
O1S C3S 1.369(5) .
C1S C2S 1.396(7) .
C3S C4S 1.379(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C21 P N Si 94.26(18) . .
C11 P N Si -26.5(2) . .
C10 P N Si -144.94(17) . .
C21 P N Cu -65.41(13) . .
C11 P N Cu 173.84(10) . .
C10 P N Cu 55.39(14) . .
C18 Si N P 161.26(18) . .
C17 Si N P -79.5(2) . .
C19 Si N P 42.9(2) . .
C18 Si N Cu -39.36(15) . .
C17 Si N Cu 79.92(14) . .
C19 Si N Cu -157.70(13) . .
N Cu N P -57.69(15) 4_565 .
I Cu N P 117.98(9) . .
N Cu N Si 137.68(6) 4_565 .
I Cu N Si -46.64(13) . .
N P C10 P -53.2(2) . 4_565
C21 P C10 P 72.00(19) . 4_565
C11 P C10 P -177.36(16) . 4_565
N P C11 C16 96.3(2) . .
C21 P C11 C16 -29.4(2) . .
C10 P C11 C16 -141.2(2) . .
N P C11 C12 -77.5(2) . .
C21 P C11 C12 156.74(19) . .
C10 P C11 C12 45.0(2) . .
C16 C11 C12 C13 0.2(4) . .
P C11 C12 C13 174.11(19) . .
C11 C12 C13 C14 -0.6(4) . .
C12 C13 C14 C15 0.5(5) . .
C13 C14 C15 C16 0.1(6) . .
C12 C11 C16 C15 0.3(5) . .
P C11 C16 C15 -173.6(3) . .
C14 C15 C16 C11 -0.5(6) . .
N P C21 C22 -1.4(2) . .
C11 P C21 C22 124.51(19) . .
C10 P C21 C22 -125.1(2) . .
N P C21 C26 -179.67(18) . .
C11 P C21 C26 -53.8(2) . .
C10 P C21 C26 56.6(2) . .
C26 C21 C22 C23 0.0(4) . .
P C21 C22 C23 -178.34(19) . .
C21 C22 C23 C24 -0.2(4) . .
C22 C23 C24 C25 0.2(4) . .
C23 C24 C25 C26 0.1(4) . .
C24 C25 C26 C21 -0.3(4) . .
C22 C21 C26 C25 0.2(4) . .
P C21 C26 C25 178.54(19) . .
C3S O1S C1S C2S 180.0 . .
C1S O1S C3S C4S 180.0 . .
