#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:13:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179682 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/04/7000499.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_7000499
loop_
_publ_author_name
'Redshaw, Carl'
'Homden, Damien'
'Hughes, David L.'
'Wright, Joseph A.'
'Elsegood, Mark R. J.'
_publ_section_title
;
 New structural motifs in chromium(iii) calix[4 and 6]arene chemistry
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1231
_journal_page_last               1242
_journal_paper_doi               10.1039/b813313a
_journal_year                    2009
_chemical_formula_moiety         'C94 H116 Cr2 N2 O8, C2 H3 N'
_chemical_formula_sum            'C96 H119 Cr2 N3 O8'
_chemical_formula_weight         1546.94
_chemical_name_common            'Compound 8'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.4736(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7763(9)
_cell_length_b                   17.4322(12)
_cell_length_c                   19.7593(14)
_cell_measurement_reflns_used    8351
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.45
_cell_volume                     4400.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6710
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39519
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        2.5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS v2007/2; Sheldrick, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.617
_refine_diff_density_min         -2.209
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         9135
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1908
_refine_ls_R_factor_gt           0.1662
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2510P)²+35.2600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4422
_refine_ls_wR_factor_ref         0.4653
_reflns_number_gt                6978
_reflns_number_total             9135
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b813313a.txt
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7000499
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.46057(13) 0.51920(11) 0.56467(8) 0.0637(6) Uani 1 1 d . . .
O1 O 0.4593(3) 0.4573(2) 0.6635(2) 0.0266(9) Uani 1 1 d . . .
O2 O 0.3228(3) 0.4693(3) 0.5451(2) 0.0335(10) Uani 1 1 d . . .
O3 O 0.4644(4) 0.5678(3) 0.4838(2) 0.0377(11) Uani 1 1 d . . .
O4 O 0.5997(3) 0.5617(3) 0.5931(2) 0.0313(10) Uani 1 1 d . . .
C1 C 0.4122(5) 0.5015(4) 0.7145(3) 0.0258(12) Uani 1 1 d . . .
C2 C 0.4734(5) 0.5512(4) 0.7508(3) 0.0299(13) Uani 1 1 d . . .
C3 C 0.4270(6) 0.5953(4) 0.8008(3) 0.0394(16) Uani 1 1 d . . .
H3 H 0.4687 0.6292 0.8273 0.047 Uiso 1 1 calc R . .
C4 C 0.3188(7) 0.5903(5) 0.8128(3) 0.0449(18) Uani 1 1 d . A .
C5 C 0.2598(6) 0.5414(4) 0.7734(4) 0.0421(17) Uani 1 1 d . . .
H5 H 0.1865 0.5385 0.7805 0.051 Uiso 1 1 calc R . .
C6 C 0.3049(5) 0.4958(4) 0.7231(3) 0.0320(14) Uani 1 1 d . . .
C7 C 0.2664(7) 0.6404(6) 0.8680(4) 0.064(2) Uani 1 1 d DU . .
C8 C 0.3423(14) 0.6948(11) 0.9016(10) 0.096(5) Uani 0.733(15) 1 d PDU A 1
H8A H 0.3743 0.7277 0.8672 0.143 Uiso 0.733(15) 1 calc PR A 1
H8B H 0.3970 0.6655 0.9251 0.143 Uiso 0.733(15) 1 calc PR A 1
H8C H 0.3050 0.7268 0.9343 0.143 Uiso 0.733(15) 1 calc PR A 1
C9 C 0.2172(14) 0.5898(9) 0.9187(7) 0.078(4) Uani 0.733(15) 1 d PDU A 1
H9A H 0.2704 0.5560 0.9386 0.117 Uiso 0.733(15) 1 calc PR A 1
H9B H 0.1628 0.5587 0.8967 0.117 Uiso 0.733(15) 1 calc PR A 1
H9C H 0.1858 0.6211 0.9543 0.117 Uiso 0.733(15) 1 calc PR A 1
C10 C 0.1814(14) 0.6892(9) 0.8351(7) 0.082(4) Uani 0.733(15) 1 d PDU A 1
H10A H 0.2129 0.7234 0.8016 0.123 Uiso 0.733(15) 1 calc PR A 1
H10B H 0.1464 0.7198 0.8699 0.123 Uiso 0.733(15) 1 calc PR A 1
H10C H 0.1301 0.6557 0.8127 0.123 Uiso 0.733(15) 1 calc PR A 1
C8X C 0.283(3) 0.7230(11) 0.8530(19) 0.078(7) Uani 0.267(15) 1 d PDU A 2
H8D H 0.2529 0.7351 0.8084 0.117 Uiso 0.267(15) 1 calc PR A 2
H8E H 0.3579 0.7343 0.8531 0.117 Uiso 0.267(15) 1 calc PR A 2
H8F H 0.2483 0.7542 0.8876 0.117 Uiso 0.267(15) 1 calc PR A 2
C9X C 0.317(3) 0.620(2) 0.9347(12) 0.080(7) Uani 0.267(15) 1 d PDU A 2
H9D H 0.3934 0.6220 0.9302 0.120 Uiso 0.267(15) 1 calc PR A 2
H9E H 0.2961 0.5680 0.9478 0.120 Uiso 0.267(15) 1 calc PR A 2
H9F H 0.2949 0.6565 0.9694 0.120 Uiso 0.267(15) 1 calc PR A 2
C10X C 0.1527(18) 0.619(2) 0.8730(19) 0.084(7) Uani 0.267(15) 1 d PDU A 2
H10D H 0.1146 0.6403 0.8339 0.125 Uiso 0.267(15) 1 calc PR A 2
H10E H 0.1238 0.6409 0.9147 0.125 Uiso 0.267(15) 1 calc PR A 2
H10F H 0.1455 0.5635 0.8736 0.125 Uiso 0.267(15) 1 calc PR A 2
C11 C 0.2361(5) 0.4486(4) 0.6767(4) 0.0367(15) Uani 1 1 d . . .
H11A H 0.1805 0.4233 0.7033 0.044 Uiso 1 1 calc R . .
H11B H 0.2784 0.4081 0.6548 0.044 Uiso 1 1 calc R . .
C12 C 0.2327(5) 0.5100(4) 0.5591(4) 0.0331(14) Uani 1 1 d . . .
C13 C 0.1866(5) 0.4994(4) 0.6228(4) 0.0338(14) Uani 1 1 d . . .
C14 C 0.0955(5) 0.5415(4) 0.6370(4) 0.0416(17) Uani 1 1 d . . .
H14 H 0.0627 0.5341 0.6795 0.050 Uiso 1 1 calc R . .
C15 C 0.0520(5) 0.5925(4) 0.5924(4) 0.0411(17) Uani 1 1 d . B .
C16 C 0.1011(5) 0.6020(4) 0.5298(4) 0.0435(17) Uani 1 1 d . . .
H16 H 0.0713 0.6366 0.4979 0.052 Uiso 1 1 calc R . .
C17 C 0.1913(5) 0.5630(4) 0.5128(4) 0.0389(16) Uani 1 1 d . . .
C18 C -0.0461(5) 0.6381(5) 0.6103(5) 0.055(2) Uani 1 1 d DU . .
C19 C -0.0159(12) 0.6974(10) 0.6672(13) 0.086(6) Uani 0.62(2) 1 d PDU B 1
H19A H -0.0778 0.7272 0.6797 0.129 Uiso 0.62(2) 1 calc PR B 1
H19B H 0.0384 0.7321 0.6503 0.129 Uiso 0.62(2) 1 calc PR B 1
H19C H 0.0108 0.6699 0.7070 0.129 Uiso 0.62(2) 1 calc PR B 1
C20 C -0.1239(10) 0.5848(10) 0.6448(12) 0.069(5) Uani 0.62(2) 1 d PDU B 1
H20A H -0.1872 0.6135 0.6562 0.104 Uiso 0.62(2) 1 calc PR B 1
H20B H -0.0922 0.5639 0.6862 0.104 Uiso 0.62(2) 1 calc PR B 1
H20C H -0.1421 0.5426 0.6141 0.104 Uiso 0.62(2) 1 calc PR B 1
C21 C -0.1019(16) 0.6752(17) 0.5496(9) 0.092(6) Uani 0.62(2) 1 d PDU B 1
H21A H -0.1645 0.7022 0.5651 0.138 Uiso 0.62(2) 1 calc PR B 1
H21B H -0.1223 0.6353 0.5170 0.138 Uiso 0.62(2) 1 calc PR B 1
H21C H -0.0546 0.7117 0.5278 0.138 Uiso 0.62(2) 1 calc PR B 1
C19X C -0.012(2) 0.7237(11) 0.6166(17) 0.075(8) Uiso 0.38(2) 1 d PDU B 2
H19D H -0.0727 0.7551 0.6287 0.112 Uiso 0.38(2) 1 calc PR B 2
H19E H 0.0161 0.7412 0.5733 0.112 Uiso 0.38(2) 1 calc PR B 2
H19F H 0.0420 0.7285 0.6519 0.112 Uiso 0.38(2) 1 calc PR B 2
C20X C -0.108(2) 0.6092(16) 0.6680(10) 0.052(6) Uiso 0.38(2) 1 d PDU B 2
H20D H -0.1684 0.6429 0.6751 0.078 Uiso 0.38(2) 1 calc PR B 2
H20E H -0.0642 0.6085 0.7089 0.078 Uiso 0.38(2) 1 calc PR B 2
H20F H -0.1326 0.5571 0.6581 0.078 Uiso 0.38(2) 1 calc PR B 2
C21X C -0.1218(19) 0.6355(17) 0.5460(10) 0.053(6) Uiso 0.38(2) 1 d PDU B 2
H21D H -0.1859 0.6642 0.5556 0.080 Uiso 0.38(2) 1 calc PR B 2
H21E H -0.1396 0.5821 0.5355 0.080 Uiso 0.38(2) 1 calc PR B 2
H21F H -0.0865 0.6586 0.5072 0.080 Uiso 0.38(2) 1 calc PR B 2
C22 C 0.2446(6) 0.5801(5) 0.4478(4) 0.0469(19) Uani 1 1 d . . .
H22A H 0.1912 0.5906 0.4124 0.056 Uiso 1 1 calc R . .
H22B H 0.2852 0.5346 0.4335 0.056 Uiso 1 1 calc R . .
C23 C 0.4248(6) 0.6391(5) 0.4736(3) 0.0439(18) Uani 1 1 d . . .
C24 C 0.3187(7) 0.6494(5) 0.4538(3) 0.0456(18) Uani 1 1 d . . .
C25 C 0.2824(7) 0.7215(6) 0.4421(4) 0.053(2) Uani 1 1 d . . .
H25 H 0.2114 0.7272 0.4283 0.063 Uiso 1 1 calc R . .
C26 C 0.3424(8) 0.7869(6) 0.4489(4) 0.055(2) Uani 1 1 d . . .
C27 C 0.4462(7) 0.7770(5) 0.4704(4) 0.051(2) Uani 1 1 d . . .
H27 H 0.4898 0.8206 0.4764 0.061 Uiso 1 1 calc R . .
C28 C 0.4871(6) 0.7032(5) 0.4832(3) 0.0427(17) Uani 1 1 d . . .
C29 C 0.3017(10) 0.8670(6) 0.4309(5) 0.071(2) Uani 1 1 d U . .
C30 C 0.1797(11) 0.8649(9) 0.4290(8) 0.103(4) Uani 1 1 d U . .
H30A H 0.1533 0.8547 0.4746 0.154 Uiso 1 1 calc R . .
H30B H 0.1562 0.8242 0.3982 0.154 Uiso 1 1 calc R . .
H30C H 0.1529 0.9144 0.4131 0.154 Uiso 1 1 calc R . .
C31 C 0.3300(10) 0.8833(7) 0.3573(6) 0.074(3) Uani 1 1 d U . .
H31A H 0.3027 0.8422 0.3284 0.112 Uiso 1 1 calc R . .
H31B H 0.4063 0.8859 0.3531 0.112 Uiso 1 1 calc R . .
H31C H 0.2993 0.9324 0.3433 0.112 Uiso 1 1 calc R . .
C32 C 0.3452(16) 0.9287(9) 0.4757(8) 0.127(6) Uani 1 1 d U . .
H32A H 0.3264 0.9182 0.5227 0.190 Uiso 1 1 calc R . .
H32B H 0.3162 0.9784 0.4619 0.190 Uiso 1 1 calc R . .
H32C H 0.4216 0.9299 0.4717 0.190 Uiso 1 1 calc R . .
C33 C 0.5993(6) 0.6980(4) 0.5083(4) 0.0416(17) Uani 1 1 d . . .
H33A H 0.6312 0.6500 0.4914 0.050 Uiso 1 1 calc R . .
H33B H 0.6399 0.7416 0.4900 0.050 Uiso 1 1 calc R . .
C34 C 0.6033(4) 0.6326(4) 0.6226(3) 0.0291(13) Uani 1 1 d . . .
C35 C 0.6055(5) 0.6993(4) 0.5848(4) 0.0328(14) Uani 1 1 d . . .
C36 C 0.6097(5) 0.7699(4) 0.6182(4) 0.0400(16) Uani 1 1 d . . .
H36 H 0.6139 0.8155 0.5920 0.048 Uiso 1 1 calc R . .
C37 C 0.6080(6) 0.7758(4) 0.6885(4) 0.0415(17) Uani 1 1 d . C .
C38 C 0.6056(6) 0.7084(4) 0.7241(4) 0.0411(16) Uani 1 1 d . . .
H38 H 0.6065 0.7109 0.7721 0.049 Uiso 1 1 calc R . .
C39 C 0.6019(4) 0.6366(4) 0.6936(3) 0.0306(13) Uani 1 1 d . . .
C40 C 0.6093(8) 0.8547(5) 0.7241(6) 0.062(2) Uani 1 1 d DU . .
C41 C 0.565(3) 0.9197(13) 0.6835(15) 0.080(7) Uani 0.60(4) 1 d PDU C 1
H41A H 0.4936 0.9066 0.6685 0.120 Uiso 0.60(4) 1 calc PR C 1
H41B H 0.6087 0.9289 0.6439 0.120 Uiso 0.60(4) 1 calc PR C 1
H41C H 0.5626 0.9660 0.7115 0.120 Uiso 0.60(4) 1 calc PR C 1
C42 C 0.7193(12) 0.8721(15) 0.7490(14) 0.072(6) Uani 0.60(4) 1 d PDU C 1
H42A H 0.7466 0.8280 0.7744 0.109 Uiso 0.60(4) 1 calc PR C 1
H42B H 0.7180 0.9172 0.7786 0.109 Uiso 0.60(4) 1 calc PR C 1
H42C H 0.7645 0.8824 0.7102 0.109 Uiso 0.60(4) 1 calc PR C 1
C43 C 0.5402(15) 0.8482(13) 0.7906(9) 0.052(4) Uani 0.60(4) 1 d PDU C 1
H43A H 0.5713 0.8102 0.8213 0.078 Uiso 0.60(4) 1 calc PR C 1
H43B H 0.4690 0.8323 0.7782 0.078 Uiso 0.60(4) 1 calc PR C 1
H43C H 0.5377 0.8982 0.8132 0.078 Uiso 0.60(4) 1 calc PR C 1
C41X C 0.531(2) 0.9062(15) 0.6871(15) 0.045(5) Uani 0.40(4) 1 d PDU C 2
H41D H 0.4596 0.8884 0.6962 0.067 Uiso 0.40(4) 1 calc PR C 2
H41E H 0.5439 0.9041 0.6384 0.067 Uiso 0.40(4) 1 calc PR C 2
H41F H 0.5389 0.9591 0.7031 0.067 Uiso 0.40(4) 1 calc PR C 2
C42X C 0.7158(17) 0.8883(19) 0.711(2) 0.090(8) Uani 0.40(4) 1 d PDU C 2
H42D H 0.7695 0.8570 0.7332 0.135 Uiso 0.40(4) 1 calc PR C 2
H42E H 0.7189 0.9408 0.7285 0.135 Uiso 0.40(4) 1 calc PR C 2
H42F H 0.7284 0.8891 0.6619 0.135 Uiso 0.40(4) 1 calc PR C 2
C43X C 0.574(3) 0.849(2) 0.7992(9) 0.072(7) Uani 0.40(4) 1 d PDU C 2
H43D H 0.5021 0.8300 0.8010 0.108 Uiso 0.40(4) 1 calc PR C 2
H43E H 0.5776 0.9001 0.8201 0.108 Uiso 0.40(4) 1 calc PR C 2
H43F H 0.6206 0.8140 0.8238 0.108 Uiso 0.40(4) 1 calc PR C 2
C44 C 0.5888(5) 0.5645(4) 0.7353(3) 0.0324(14) Uani 1 1 d . . .
H44A H 0.6289 0.5694 0.7782 0.039 Uiso 1 1 calc R . .
H44B H 0.6168 0.5200 0.7102 0.039 Uiso 1 1 calc R . .
C45 C 0.4898(7) 0.3821(4) 0.6870(4) 0.0453(18) Uani 1 1 d . . .
H45A H 0.4271 0.3521 0.6976 0.068 Uiso 1 1 calc R . .
H45B H 0.5335 0.3871 0.7278 0.068 Uiso 1 1 calc R . .
H45C H 0.5296 0.3559 0.6517 0.068 Uiso 1 1 calc R . .
N1 N 0.3858(7) 0.6111(6) 0.6116(5) 0.070(2) Uani 1 1 d . . .
C46 C 0.3382(8) 0.6781(8) 0.6307(5) 0.066(3) Uani 1 1 d . . .
C47 C 0.2976(11) 0.7481(11) 0.6518(8) 0.108(6) Uani 1 1 d . . .
H47A H 0.2352 0.7392 0.6793 0.161 Uiso 1 1 calc R . .
H47B H 0.2788 0.7791 0.6122 0.161 Uiso 1 1 calc R . .
H47C H 0.3504 0.7754 0.6790 0.161 Uiso 1 1 calc R . .
N2 N 0.144(3) 0.884(2) 0.646(2) 0.162(12) Uani 0.50 1 d PDU . .
C48 C 0.071(2) 0.9104(13) 0.6153(12) 0.096(7) Uani 0.50 1 d PDU . .
C49 C -0.039(3) 0.9314(15) 0.5943(16) 0.129(11) Uani 0.50 1 d PDU . .
H49A H -0.0504 0.9865 0.6013 0.193 Uiso 0.50 1 calc PR . .
H49B H -0.0894 0.9023 0.6215 0.193 Uiso 0.50 1 calc PR . .
H49C H -0.0498 0.9192 0.5463 0.193 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'
Cr Cr 0.3209 0.6236 '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
_geom_angle_publ_flag
O3 Cr1 O2 93.7(2) . . ?
O3 Cr1 O4 92.5(2) . . ?
O2 Cr1 O4 173.7(2) . . ?
O3 Cr1 O3 85.3(2) . 3_666 ?
O2 Cr1 O3 90.1(2) . 3_666 ?
O4 Cr1 O3 89.3(2) . 3_666 ?
O3 Cr1 N1 92.8(3) . . ?
O2 Cr1 N1 90.8(3) . . ?
O4 Cr1 N1 90.0(3) . . ?
O3 Cr1 N1 177.9(3) 3_666 . ?
O3 Cr1 O1 178.5(2) . . ?
O2 Cr1 O1 86.89(19) . . ?
O4 Cr1 O1 86.93(18) . . ?
O3 Cr1 O1 93.32(18) 3_666 . ?
N1 Cr1 O1 88.6(3) . . ?
O3 Cr1 Cr1 45.75(15) . 3_666 ?
O2 Cr1 Cr1 92.42(15) . 3_666 ?
O4 Cr1 Cr1 91.08(15) . 3_666 ?
O3 Cr1 Cr1 39.53(14) 3_666 3_666 ?
N1 Cr1 Cr1 138.5(3) . 3_666 ?
O1 Cr1 Cr1 132.85(14) . 3_666 ?
C1 O1 C45 112.5(5) . . ?
C1 O1 Cr1 111.6(3) . . ?
C45 O1 Cr1 135.8(4) . . ?
C12 O2 Cr1 118.1(4) . . ?
C23 O3 Cr1 123.2(4) . . ?
C23 O3 Cr1 142.1(4) . 3_666 ?
Cr1 O3 Cr1 94.7(2) . 3_666 ?
C34 O4 Cr1 118.7(4) . . ?
C2 C1 C6 122.9(5) . . ?
C2 C1 O1 118.5(5) . . ?
C6 C1 O1 118.5(6) . . ?
C1 C2 C3 118.5(6) . . ?
C1 C2 C44 122.7(5) . . ?
C3 C2 C44 118.6(6) . . ?
C2 C3 C4 120.8(7) . . ?
C5 C4 C3 118.6(6) . . ?
C5 C4 C7 120.6(7) . . ?
C3 C4 C7 120.9(8) . . ?
C4 C5 C6 121.8(7) . . ?
C1 C6 C5 117.3(7) . . ?
C1 C6 C11 122.4(5) . . ?
C5 C6 C11 120.0(6) . . ?
C9 C7 C8X 140.8(14) . . ?
C9 C7 C10X 52.7(18) . . ?
C8X C7 C10X 113(2) . . ?
C9 C7 C9X 56.6(16) . . ?
C8X C7 C9X 110.1(18) . . ?
C10X C7 C9X 107.2(17) . . ?
C9 C7 C8 110.7(11) . . ?
C8X C7 C8 52.1(17) . . ?
C10X C7 C8 138.1(15) . . ?
C9X C7 C8 59.6(17) . . ?
C9 C7 C10 108.5(10) . . ?
C8X C7 C10 58(2) . . ?
C10X C7 C10 58.4(17) . . ?
C9X C7 C10 143.8(15) . . ?
C8 C7 C10 106.9(13) . . ?
C9 C7 C4 109.2(9) . . ?
C8X C7 C4 110.0(13) . . ?
C10X C7 C4 109.4(14) . . ?
C9X C7 C4 107.3(15) . . ?
C8 C7 C4 112.6(8) . . ?
C10 C7 C4 108.9(8) . . ?
C6 C11 C13 110.1(5) . . ?
O2 C12 C17 121.3(6) . . ?
O2 C12 C13 117.8(6) . . ?
C17 C12 C13 120.8(6) . . ?
C14 C13 C12 117.7(7) . . ?
C14 C13 C11 120.3(7) . . ?
C12 C13 C11 122.0(5) . . ?
C15 C14 C13 122.9(7) . . ?
C14 C15 C16 117.6(6) . . ?
C14 C15 C18 121.2(7) . . ?
C16 C15 C18 121.2(7) . . ?
C17 C16 C15 122.5(7) . . ?
C16 C17 C12 118.5(7) . . ?
C16 C17 C22 120.0(7) . . ?
C12 C17 C22 121.4(6) . . ?
C20X C18 C15 116.5(13) . . ?
C20 C18 C15 109.0(8) . . ?
C20X C18 C21 119.8(15) . . ?
C20 C18 C21 107.8(12) . . ?
C15 C18 C21 114.5(9) . . ?
C20X C18 C19X 114.5(15) . . ?
C20 C18 C19X 136.9(14) . . ?
C15 C18 C19X 106.6(13) . . ?
C21 C18 C19X 77.7(18) . . ?
C20X C18 C19 78.7(13) . . ?
C20 C18 C19 103.8(12) . . ?
C15 C18 C19 108.1(7) . . ?
C21 C18 C19 113.1(14) . . ?
C20X C18 C21X 106.3(13) . . ?
C20 C18 C21X 86.9(12) . . ?
C15 C18 C21X 107.1(12) . . ?
C19X C18 C21X 105.0(16) . . ?
C19 C18 C21X 137.2(14) . . ?
C17 C22 C24 112.1(6) . . ?
O3 C23 C28 120.4(7) . . ?
O3 C23 C24 120.8(8) . . ?
C28 C23 C24 118.8(8) . . ?
C25 C24 C23 119.2(9) . . ?
C25 C24 C22 120.3(8) . . ?
C23 C24 C22 120.5(7) . . ?
C24 C25 C26 124.0(9) . . ?
C25 C26 C27 116.9(8) . . ?
C25 C26 C29 122.9(9) . . ?
C27 C26 C29 120.1(10) . . ?
C26 C27 C28 121.0(9) . . ?
C23 C28 C27 120.0(8) . . ?
C23 C28 C33 122.5(7) . . ?
C27 C28 C33 117.5(8) . . ?
C32 C29 C31 109.8(12) . . ?
C32 C29 C26 113.2(9) . . ?
C31 C29 C26 107.9(9) . . ?
C32 C29 C30 113.4(12) . . ?
C31 C29 C30 103.1(10) . . ?
C26 C29 C30 108.7(10) . . ?
C35 C33 C28 111.6(5) . . ?
O4 C34 C35 122.1(6) . . ?
O4 C34 C39 118.0(6) . . ?
C35 C34 C39 119.9(6) . . ?
C34 C35 C36 119.1(7) . . ?
C34 C35 C33 121.7(6) . . ?
C36 C35 C33 119.1(6) . . ?
C37 C36 C35 122.4(7) . . ?
C38 C37 C36 116.7(7) . . ?
C38 C37 C40 122.0(8) . . ?
C36 C37 C40 121.4(7) . . ?
C37 C38 C39 123.5(7) . . ?
C38 C39 C34 118.4(6) . . ?
C38 C39 C44 121.1(6) . . ?
C34 C39 C44 120.4(5) . . ?
C41 C40 C42X 87.2(19) . . ?
C41 C40 C42 111.7(15) . . ?
C42X C40 C41X 106.1(17) . . ?
C42 C40 C41X 129.8(16) . . ?
C41 C40 C37 115.2(14) . . ?
C42X C40 C37 105.8(16) . . ?
C42 C40 C37 109.4(11) . . ?
C41X C40 C37 107.5(13) . . ?
C41 C40 C43X 117(2) . . ?
C42X C40 C43X 117.3(18) . . ?
C41X C40 C43X 107.4(16) . . ?
C37 C40 C43X 112.2(17) . . ?
C41 C40 C43 106.6(14) . . ?
C42 C40 C43 105.4(12) . . ?
C41X C40 C43 94.1(15) . . ?
C37 C40 C43 108.0(11) . . ?
C39 C44 C2 110.2(5) . . ?
C46 N1 Cr1 169.2(8) . . ?
N1 C46 C47 175.4(10) . . ?
N2 C48 C49 162(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O3 1.810(5) . ?
Cr1 O2 1.999(5) . ?
Cr1 O4 2.002(5) . ?
Cr1 O3 2.038(5) 3_666 ?
Cr1 N1 2.087(9) . ?
Cr1 O1 2.231(5) . ?
Cr1 Cr1 2.835(3) 3_666 ?
O1 C1 1.408(6) . ?
O1 C45 1.444(8) . ?
O2 C12 1.381(7) . ?
O3 C23 1.356(10) . ?
O3 Cr1 2.038(5) 3_666 ?
O4 C34 1.368(8) . ?
C1 C2 1.367(9) . ?
C1 C6 1.387(9) . ?
C2 C3 1.388(9) . ?
C2 C44 1.526(9) . ?
C3 C4 1.406(11) . ?
C4 C5 1.375(12) . ?
C4 C7 1.554(9) . ?
C5 C6 1.399(9) . ?
C6 C11 1.510(10) . ?
C7 C9 1.477(16) . ?
C7 C8X 1.486(18) . ?
C7 C10X 1.502(18) . ?
C7 C9X 1.50(2) . ?
C7 C8 1.507(15) . ?
C7 C10 1.522(15) . ?
C11 C13 1.519(10) . ?
C12 C17 1.400(10) . ?
C12 C13 1.406(10) . ?
C13 C14 1.406(9) . ?
C14 C15 1.368(11) . ?
C15 C16 1.400(12) . ?
C15 C18 1.528(9) . ?
C16 C17 1.382(10) . ?
C17 C22 1.490(12) . ?
C18 C20X 1.481(19) . ?
C18 C20 1.524(16) . ?
C18 C21 1.534(15) . ?
C18 C19X 1.559(17) . ?
C18 C19 1.573(14) . ?
C18 C21X 1.592(16) . ?
C22 C24 1.538(13) . ?
C23 C28 1.385(12) . ?
C23 C24 1.419(11) . ?
C24 C25 1.359(12) . ?
C25 C26 1.380(14) . ?
C26 C27 1.399(13) . ?
C26 C29 1.532(13) . ?
C27 C28 1.410(12) . ?
C28 C33 1.517(11) . ?
C29 C32 1.496(19) . ?
C29 C31 1.528(15) . ?
C29 C30 1.559(19) . ?
C33 C35 1.514(10) . ?
C34 C35 1.381(10) . ?
C34 C39 1.406(9) . ?
C35 C36 1.397(10) . ?
C36 C37 1.392(12) . ?
C37 C38 1.370(11) . ?
C37 C40 1.546(11) . ?
C38 C39 1.389(9) . ?
C39 C44 1.513(10) . ?
C40 C41 1.498(17) . ?
C40 C42X 1.51(2) . ?
C40 C42 1.517(17) . ?
C40 C41X 1.527(18) . ?
C40 C43X 1.56(2) . ?
C40 C43 1.592(19) . ?
N1 C46 1.371(17) . ?
C46 C47 1.39(2) . ?
N2 C48 1.193(19) . ?
C48 C49 1.509(19) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cr1 O1 C1 -91.0(4) . . . . ?
O4 Cr1 O1 C1 90.0(4) . . . . ?
O3 Cr1 O1 C1 179.1(4) 3_666 . . . ?
N1 Cr1 O1 C1 -0.1(4) . . . . ?
Cr1 Cr1 O1 C1 178.6(3) 3_666 . . . ?
O2 Cr1 O1 C45 85.1(6) . . . . ?
O4 Cr1 O1 C45 -93.9(6) . . . . ?
O3 Cr1 O1 C45 -4.8(6) 3_666 . . . ?
N1 Cr1 O1 C45 176.0(7) . . . . ?
Cr1 Cr1 O1 C45 -5.3(7) 3_666 . . . ?
O3 Cr1 O2 C12 -85.7(5) . . . . ?
O3 Cr1 O2 C12 -171.0(5) 3_666 . . . ?
N1 Cr1 O2 C12 7.1(5) . . . . ?
O1 Cr1 O2 C12 95.7(5) . . . . ?
Cr1 Cr1 O2 C12 -131.5(5) 3_666 . . . ?
O2 Cr1 O3 C23 90.5(6) . . . . ?
O4 Cr1 O3 C23 -90.6(6) . . . . ?
O3 Cr1 O3 C23 -179.7(7) 3_666 . . . ?
N1 Cr1 O3 C23 -0.5(6) . . . . ?
Cr1 Cr1 O3 C23 -179.7(7) 3_666 . . . ?
O2 Cr1 O3 Cr1 -89.8(2) . . . 3_666 ?
O4 Cr1 O3 Cr1 89.1(2) . . . 3_666 ?
O3 Cr1 O3 Cr1 0.0 3_666 . . 3_666 ?
N1 Cr1 O3 Cr1 179.2(3) . . . 3_666 ?
O3 Cr1 O4 C34 85.4(5) . . . . ?
O3 Cr1 O4 C34 170.7(5) 3_666 . . . ?
N1 Cr1 O4 C34 -7.3(5) . . . . ?
O1 Cr1 O4 C34 -95.9(4) . . . . ?
Cr1 Cr1 O4 C34 131.2(4) 3_666 . . . ?
C45 O1 C1 C2 95.1(7) . . . . ?
Cr1 O1 C1 C2 -87.8(6) . . . . ?
C45 O1 C1 C6 -88.4(7) . . . . ?
Cr1 O1 C1 C6 88.6(6) . . . . ?
C6 C1 C2 C3 3.3(10) . . . . ?
O1 C1 C2 C3 179.6(6) . . . . ?
C6 C1 C2 C44 -172.3(6) . . . . ?
O1 C1 C2 C44 4.0(9) . . . . ?
C1 C2 C3 C4 -1.6(10) . . . . ?
C44 C2 C3 C4 174.2(6) . . . . ?
C2 C3 C4 C5 -0.7(11) . . . . ?
C2 C3 C4 C7 -179.1(7) . . . . ?
C3 C4 C5 C6 1.3(11) . . . . ?
C7 C4 C5 C6 179.8(7) . . . . ?
C2 C1 C6 C5 -2.6(9) . . . . ?
O1 C1 C6 C5 -178.9(6) . . . . ?
C2 C1 C6 C11 171.7(6) . . . . ?
O1 C1 C6 C11 -4.5(9) . . . . ?
C4 C5 C6 C1 0.3(10) . . . . ?
C4 C5 C6 C11 -174.3(7) . . . . ?
C5 C4 C7 C9 61.5(12) . . . . ?
C3 C4 C7 C9 -120.1(11) . . . . ?
C5 C4 C7 C8X -119(2) . . . . ?
C3 C4 C7 C8X 60(2) . . . . ?
C5 C4 C7 C10X 5(2) . . . . ?
C3 C4 C7 C10X -176.2(19) . . . . ?
C5 C4 C7 C9X 121.3(18) . . . . ?
C3 C4 C7 C9X -60.2(18) . . . . ?
C5 C4 C7 C8 -175.1(12) . . . . ?
C3 C4 C7 C8 3.3(15) . . . . ?
C5 C4 C7 C10 -56.8(12) . . . . ?
C3 C4 C7 C10 121.7(11) . . . . ?
C1 C6 C11 C13 -96.8(7) . . . . ?
C5 C6 C11 C13 77.4(7) . . . . ?
Cr1 O2 C12 C17 84.0(7) . . . . ?
Cr1 O2 C12 C13 -92.9(6) . . . . ?
O2 C12 C13 C14 179.5(6) . . . . ?
C17 C12 C13 C14 2.6(10) . . . . ?
O2 C12 C13 C11 3.3(9) . . . . ?
C17 C12 C13 C11 -173.6(6) . . . . ?
C6 C11 C13 C14 -82.9(7) . . . . ?
C6 C11 C13 C12 93.2(7) . . . . ?
C12 C13 C14 C15 -1.3(11) . . . . ?
C11 C13 C14 C15 175.0(7) . . . . ?
C13 C14 C15 C16 0.5(11) . . . . ?
C13 C14 C15 C18 -179.0(7) . . . . ?
C14 C15 C16 C17 -1.1(11) . . . . ?
C18 C15 C16 C17 178.4(7) . . . . ?
C15 C16 C17 C12 2.4(11) . . . . ?
C15 C16 C17 C22 -175.1(7) . . . . ?
O2 C12 C17 C16 -179.9(6) . . . . ?
C13 C12 C17 C16 -3.1(10) . . . . ?
O2 C12 C17 C22 -2.4(10) . . . . ?
C13 C12 C17 C22 174.3(6) . . . . ?
C14 C15 C18 C20X -17.0(15) . . . . ?
C16 C15 C18 C20X 163.5(13) . . . . ?
C14 C15 C18 C20 -43.1(13) . . . . ?
C16 C15 C18 C20 137.4(12) . . . . ?
C14 C15 C18 C21 -163.9(15) . . . . ?
C16 C15 C18 C21 16.6(17) . . . . ?
C14 C15 C18 C19X 112.3(15) . . . . ?
C16 C15 C18 C19X -67.2(15) . . . . ?
C14 C15 C18 C19 69.1(14) . . . . ?
C16 C15 C18 C19 -110.4(13) . . . . ?
C14 C15 C18 C21X -135.7(13) . . . . ?
C16 C15 C18 C21X 44.8(14) . . . . ?
C16 C17 C22 C24 84.3(8) . . . . ?
C12 C17 C22 C24 -93.1(8) . . . . ?
Cr1 O3 C23 C28 90.1(7) . . . . ?
Cr1 O3 C23 C28 -89.4(9) 3_666 . . . ?
Cr1 O3 C23 C24 -89.2(7) . . . . ?
Cr1 O3 C23 C24 91.3(9) 3_666 . . . ?
O3 C23 C24 C25 -178.0(6) . . . . ?
C28 C23 C24 C25 2.7(10) . . . . ?
O3 C23 C24 C22 3.8(9) . . . . ?
C28 C23 C24 C22 -175.4(6) . . . . ?
C17 C22 C24 C25 -88.9(8) . . . . ?
C17 C22 C24 C23 89.2(8) . . . . ?
C23 C24 C25 C26 -0.8(11) . . . . ?
C22 C24 C25 C26 177.4(7) . . . . ?
C24 C25 C26 C27 -1.1(12) . . . . ?
C24 C25 C26 C29 175.9(8) . . . . ?
C25 C26 C27 C28 1.0(11) . . . . ?
C29 C26 C27 C28 -176.0(7) . . . . ?
O3 C23 C28 C27 177.9(6) . . . . ?
C24 C23 C28 C27 -2.8(9) . . . . ?
O3 C23 C28 C33 -3.0(9) . . . . ?
C24 C23 C28 C33 176.3(6) . . . . ?
C26 C27 C28 C23 0.9(10) . . . . ?
C26 C27 C28 C33 -178.2(6) . . . . ?
C25 C26 C29 C32 146.1(13) . . . . ?
C27 C26 C29 C32 -37.0(15) . . . . ?
C25 C26 C29 C31 -92.1(11) . . . . ?
C27 C26 C29 C31 84.8(11) . . . . ?
C25 C26 C29 C30 19.1(13) . . . . ?
C27 C26 C29 C30 -164.1(9) . . . . ?
C23 C28 C33 C35 -88.2(8) . . . . ?
C27 C28 C33 C35 90.8(7) . . . . ?
Cr1 O4 C34 C35 -84.3(6) . . . . ?
Cr1 O4 C34 C39 93.9(6) . . . . ?
O4 C34 C35 C36 -179.7(5) . . . . ?
C39 C34 C35 C36 2.1(9) . . . . ?
O4 C34 C35 C33 2.7(9) . . . . ?
C39 C34 C35 C33 -175.5(6) . . . . ?
C28 C33 C35 C34 90.8(8) . . . . ?
C28 C33 C35 C36 -86.8(8) . . . . ?
C34 C35 C36 C37 -2.3(10) . . . . ?
C33 C35 C36 C37 175.3(6) . . . . ?
C35 C36 C37 C38 2.2(10) . . . . ?
C35 C36 C37 C40 -178.1(7) . . . . ?
C36 C37 C38 C39 -1.8(11) . . . . ?
C40 C37 C38 C39 178.4(7) . . . . ?
C37 C38 C39 C34 1.7(10) . . . . ?
C37 C38 C39 C44 -174.1(6) . . . . ?
O4 C34 C39 C38 180.0(5) . . . . ?
C35 C34 C39 C38 -1.8(9) . . . . ?
O4 C34 C39 C44 -4.2(8) . . . . ?
C35 C34 C39 C44 174.0(5) . . . . ?
C38 C37 C40 C41 -153.7(17) . . . . ?
C36 C37 C40 C41 26.6(19) . . . . ?
C38 C37 C40 C42X 112(2) . . . . ?
C36 C37 C40 C42X -68(2) . . . . ?
C38 C37 C40 C42 79.5(16) . . . . ?
C36 C37 C40 C42 -100.3(15) . . . . ?
C38 C37 C40 C41X -135.2(15) . . . . ?
C36 C37 C40 C41X 45.1(16) . . . . ?
C38 C37 C40 C43X -17.2(18) . . . . ?
C36 C37 C40 C43X 163.0(17) . . . . ?
C38 C37 C40 C43 -34.7(12) . . . . ?
C36 C37 C40 C43 145.5(10) . . . . ?
C38 C39 C44 C2 82.9(7) . . . . ?
C34 C39 C44 C2 -92.7(7) . . . . ?
C1 C2 C44 C39 98.7(7) . . . . ?
C3 C2 C44 C39 -76.9(7) . . . . ?
O3 Cr1 N1 C46 -2(4) . . . . ?
O2 Cr1 N1 C46 -95(4) . . . . ?
O4 Cr1 N1 C46 91(4) . . . . ?
O1 Cr1 N1 C46 178(4) . . . . ?
Cr1 Cr1 N1 C46 -1(4) 3_666 . . . ?
