#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/73/2227370.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_2227370
loop_
_publ_author_name
'Peulecke, Normen'
'Peitz, Stephan'
'Müller, Bernd H.'
'Spannenberg, Anke'
'Rosenthal, Uwe'
_publ_section_title
;
 [2,2-Bis(diphenylphosphanyl)propane-κ²P,P']tetracarbonylchromium(0)
 dichloromethane monosolvate
;
_journal_coeditor_code           CV2782
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1495
_journal_paper_doi               10.1107/S1600536810043692
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cr (C27 H26 P2) (C O)4] , C H2 Cl2'
_chemical_formula_moiety         'C31 H26 Cr O4 P2, C H2 Cl2'
_chemical_formula_sum            'C32 H28 Cl2 Cr O4 P2'
_chemical_formula_weight         661.38
_chemical_name_systematic
;
[2,2-Bis(diphenylphosphanyl)propane-
κ²P,P']tetracarbonylchromium dichloromethane monosolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                99.811(4)
_cell_angle_beta                 94.856(4)
_cell_angle_gamma                93.020(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9998(5)
_cell_length_b                   9.4895(5)
_cell_length_c                   18.3178(9)
_cell_measurement_reflns_used    4481
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.15
_cell_volume                     1532.40(14)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25497
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.8338
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.646
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0478P)²+0.3172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                5824
_reflns_number_total             7051
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2782.cif
_cod_data_source_block           I
_cod_database_code               2227370
_cod_database_fobs_code          2227370
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 1.01536(18) 0.20775(19) 0.18509(10) 0.0267(4) Uani d . 1 . .
C C2 0.76174(18) 0.13420(18) 0.22785(10) 0.0248(3) Uani d . 1 . .
C C3 0.96144(18) 0.26041(19) 0.33115(10) 0.0277(4) Uani d . 1 . .
C C4 1.02766(18) 0.46144(19) 0.25461(10) 0.0270(4) Uani d . 1 . .
C C5 0.57483(17) 0.44246(17) 0.20067(9) 0.0216(3) Uani d . 1 . .
C C6 0.45608(17) 0.31571(19) 0.19234(10) 0.0259(3) Uani d . 1 . .
H H6A 0.3801 0.3405 0.2268 0.039 Uiso calc R 1 . .
H H6B 0.5041 0.2307 0.2038 0.039 Uiso calc R 1 . .
H H6C 0.4087 0.2955 0.1411 0.039 Uiso calc R 1 . .
C C7 0.49660(19) 0.57332(19) 0.18302(10) 0.0277(4) Uani d . 1 . .
H H7A 0.4490 0.5525 0.1319 0.041 Uiso calc R 1 . .
H H7B 0.5702 0.6552 0.1883 0.041 Uiso calc R 1 . .
H H7C 0.4204 0.5963 0.2176 0.041 Uiso calc R 1 . .
C C8 0.80565(17) 0.54283(18) 0.10865(10) 0.0241(3) Uani d . 1 . .
C C9 0.81566(19) 0.5386(2) 0.03282(11) 0.0300(4) Uani d . 1 . .
H H9 0.7802 0.4547 -0.0017 0.036 Uiso calc R 1 . .
C C10 0.8776(2) 0.6569(2) 0.00739(12) 0.0369(4) Uani d . 1 . .
H H10 0.8841 0.6533 -0.0444 0.044 Uiso calc R 1 . .
C C11 0.9293(2) 0.7788(2) 0.05695(13) 0.0381(5) Uani d . 1 . .
H H11 0.9712 0.8592 0.0393 0.046 Uiso calc R 1 . .
C C12 0.9204(2) 0.7847(2) 0.13238(13) 0.0356(4) Uani d . 1 . .
H H12 0.9558 0.8691 0.1665 0.043 Uiso calc R 1 . .
C C13 0.85938(18) 0.66646(19) 0.15817(11) 0.0292(4) Uani d . 1 . .
H H13 0.8544 0.6703 0.2101 0.035 Uiso calc R 1 . .
C C14 0.66313(18) 0.26334(18) 0.06079(9) 0.0240(3) Uani d . 1 . .
C C15 0.73759(18) 0.14068(19) 0.03805(10) 0.0264(4) Uani d . 1 . .
H H15 0.8206 0.1186 0.0687 0.032 Uiso calc R 1 . .
C C16 0.6919(2) 0.0507(2) -0.02876(11) 0.0316(4) Uani d . 1 . .
H H16 0.7451 -0.0313 -0.0443 0.038 Uiso calc R 1 . .
C C17 0.5691(2) 0.0798(2) -0.07279(10) 0.0325(4) Uani d . 1 . .
H H17 0.5380 0.0180 -0.1186 0.039 Uiso calc R 1 . .
C C18 0.4914(2) 0.1991(2) -0.05008(10) 0.0309(4) Uani d . 1 . .
H H18 0.4053 0.2176 -0.0797 0.037 Uiso calc R 1 . .
C C19 0.53874(19) 0.2914(2) 0.01568(10) 0.0282(4) Uani d . 1 . .
H H19 0.4864 0.3744 0.0303 0.034 Uiso calc R 1 . .
C C20 0.74847(18) 0.63022(18) 0.34037(9) 0.0241(3) Uani d . 1 . .
C C21 0.6667(2) 0.74999(19) 0.33735(11) 0.0321(4) Uani d . 1 . .
H H21 0.5747 0.7410 0.3069 0.039 Uiso calc R 1 . .
C C22 0.7189(3) 0.8825(2) 0.37862(12) 0.0403(5) Uani d . 1 . .
H H22 0.6632 0.9640 0.3755 0.048 Uiso calc R 1 . .
C C23 0.8507(2) 0.8967(2) 0.42396(12) 0.0410(5) Uani d . 1 . .
H H23 0.8867 0.9880 0.4513 0.049 Uiso calc R 1 . .
C C24 0.9306(2) 0.7781(2) 0.42962(11) 0.0367(4) Uani d . 1 . .
H H24 1.0197 0.7869 0.4623 0.044 Uiso calc R 1 . .
C C25 0.88029(19) 0.6458(2) 0.38738(10) 0.0289(4) Uani d . 1 . .
H H25 0.9367 0.5648 0.3906 0.035 Uiso calc R 1 . .
C C26 0.56456(17) 0.39289(17) 0.35684(9) 0.0232(3) Uani d . 1 . .
C C27 0.44294(19) 0.4714(2) 0.37624(11) 0.0309(4) Uani d . 1 . .
H H27 0.4247 0.5550 0.3557 0.037 Uiso calc R 1 . .
C C28 0.3486(2) 0.4280(2) 0.42524(12) 0.0377(4) Uani d . 1 . .
H H28 0.2654 0.4816 0.4380 0.045 Uiso calc R 1 . .
C C29 0.3749(2) 0.3072(2) 0.45557(11) 0.0381(5) Uani d . 1 . .
H H29 0.3098 0.2776 0.4892 0.046 Uiso calc R 1 . .
C C30 0.4951(2) 0.2296(2) 0.43722(11) 0.0371(4) Uani d . 1 . .
H H30 0.5133 0.1469 0.4585 0.045 Uiso calc R 1 . .
C C31 0.5902(2) 0.27148(19) 0.38763(10) 0.0293(4) Uani d . 1 . .
H H31 0.6728 0.2170 0.3748 0.035 Uiso calc R 1 . .
C C32 0.2113(3) 0.9291(3) 0.33113(16) 0.0622(7) Uani d . 1 . .
H H32A 0.1155 0.8720 0.3145 0.075 Uiso calc R 1 . .
H H32B 0.1881 1.0281 0.3515 0.075 Uiso calc R 1 . .
Cl Cl1 0.30771(6) 0.85575(7) 0.40154(4) 0.05184(15) Uani d . 1 . .
Cl Cl2 0.31373(9) 0.93219(10) 0.25513(5) 0.0796(2) Uani d . 1 . .
Cr Cr1 0.88203(3) 0.30677(3) 0.242280(15) 0.02031(8) Uani d . 1 . .
O O1 1.09906(15) 0.14688(15) 0.14916(8) 0.0396(3) Uani d . 1 . .
O O2 0.69755(15) 0.02391(13) 0.21958(8) 0.0353(3) Uani d . 1 . .
O O3 1.00875(16) 0.22861(17) 0.38596(8) 0.0426(3) Uani d . 1 . .
O O4 1.12468(14) 0.54764(15) 0.26147(9) 0.0401(3) Uani d . 1 . .
P P1 0.73655(4) 0.38536(4) 0.14524(2) 0.02048(10) Uani d . 1 . .
P P2 0.69140(4) 0.44708(4) 0.29237(2) 0.01995(10) Uani d . 1 . .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 Cr1 . . 179.44(16) ?
O2 C2 Cr1 . . 175.10(15) ?
O3 C3 Cr1 . . 178.39(16) ?
O4 C4 Cr1 . . 174.55(16) ?
C7 C5 C6 . . 108.25(13) ?
C7 C5 P1 . . 117.15(11) ?
C6 C5 P1 . . 109.61(12) ?
C7 C5 P2 . . 121.62(12) ?
C6 C5 P2 . . 106.88(11) ?
P1 C5 P2 . . 92.07(7) ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C5 C7 H7A . . 109.5 ?
C5 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C5 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C13 C8 C9 . . 118.82(15) ?
C13 C8 P1 . . 119.29(13) ?
C9 C8 P1 . . 121.74(14) ?
C8 C9 C10 . . 120.26(19) ?
C8 C9 H9 . . 119.9 ?
C10 C9 H9 . . 119.9 ?
C11 C10 C9 . . 120.31(19) ?
C11 C10 H10 . . 119.8 ?
C9 C10 H10 . . 119.8 ?
C10 C11 C12 . . 120.14(17) ?
C10 C11 H11 . . 119.9 ?
C12 C11 H11 . . 119.9 ?
C11 C12 C13 . . 119.81(19) ?
C11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
C8 C13 C12 . . 120.66(18) ?
C8 C13 H13 . . 119.7 ?
C12 C13 H13 . . 119.7 ?
C15 C14 C19 . . 118.54(16) ?
C15 C14 P1 . . 118.92(13) ?
C19 C14 P1 . . 122.46(14) ?
C16 C15 C14 . . 120.68(17) ?
C16 C15 H15 . . 119.7 ?
C14 C15 H15 . . 119.7 ?
C17 C16 C15 . . 120.13(18) ?
C17 C16 H16 . . 119.9 ?
C15 C16 H16 . . 119.9 ?
C16 C17 C18 . . 119.94(17) ?
C16 C17 H17 . . 120.0 ?
C18 C17 H17 . . 120.0 ?
C19 C18 C17 . . 120.19(17) ?
C19 C18 H18 . . 119.9 ?
C17 C18 H18 . . 119.9 ?
C18 C19 C14 . . 120.47(17) ?
C18 C19 H19 . . 119.8 ?
C14 C19 H19 . . 119.8 ?
C25 C20 C21 . . 118.50(16) ?
C25 C20 P2 . . 115.71(13) ?
C21 C20 P2 . . 125.64(13) ?
C22 C21 C20 . . 120.37(18) ?
C22 C21 H21 . . 119.8 ?
C20 C21 H21 . . 119.8 ?
C23 C22 C21 . . 120.44(19) ?
C23 C22 H22 . . 119.8 ?
C21 C22 H22 . . 119.8 ?
C22 C23 C24 . . 119.97(18) ?
C22 C23 H23 . . 120.0 ?
C24 C23 H23 . . 120.0 ?
C23 C24 C25 . . 119.77(19) ?
C23 C24 H24 . . 120.1 ?
C25 C24 H24 . . 120.1 ?
C24 C25 C20 . . 120.90(18) ?
C24 C25 H25 . . 119.6 ?
C20 C25 H25 . . 119.6 ?
C31 C26 C27 . . 119.18(15) ?
C31 C26 P2 . . 119.40(13) ?
C27 C26 P2 . . 121.43(13) ?
C28 C27 C26 . . 120.27(17) ?
C28 C27 H27 . . 119.9 ?
C26 C27 H27 . . 119.9 ?
C29 C28 C27 . . 120.18(19) ?
C29 C28 H28 . . 119.9 ?
C27 C28 H28 . . 119.9 ?
C30 C29 C28 . . 120.01(17) ?
C30 C29 H29 . . 120.0 ?
C28 C29 H29 . . 120.0 ?
C29 C30 C31 . . 120.39(18) ?
C29 C30 H30 . . 119.8 ?
C31 C30 H30 . . 119.8 ?
C26 C31 C30 . . 119.97(18) ?
C26 C31 H31 . . 120.0 ?
C30 C31 H31 . . 120.0 ?
Cl2 C32 Cl1 . . 112.25(14) ?
Cl2 C32 H32A . . 109.2 ?
Cl1 C32 H32A . . 109.2 ?
Cl2 C32 H32B . . 109.2 ?
Cl1 C32 H32B . . 109.2 ?
H32A C32 H32B . . 107.9 ?
C1 Cr1 C3 . . 94.87(8) ?
C1 Cr1 C2 . . 87.32(7) ?
C3 Cr1 C2 . . 87.49(7) ?
C1 Cr1 C4 . . 84.72(7) ?
C3 Cr1 C4 . . 89.19(7) ?
C2 Cr1 C4 . . 171.09(7) ?
C1 Cr1 P1 . . 98.01(6) ?
C3 Cr1 P1 . . 166.91(6) ?
C2 Cr1 P1 . . 90.76(5) ?
C4 Cr1 P1 . . 94.31(5) ?
C1 Cr1 P2 . . 168.24(6) ?
C3 Cr1 P2 . . 96.88(6) ?
C2 Cr1 P2 . . 93.54(5) ?
C4 Cr1 P2 . . 95.07(5) ?
P1 Cr1 P2 . . 70.265(16) ?
C14 P1 C8 . . 102.23(8) ?
C14 P1 C5 . . 108.57(7) ?
C8 P1 C5 . . 106.88(7) ?
C14 P1 Cr1 . . 121.91(6) ?
C8 P1 Cr1 . . 119.29(6) ?
C5 P1 Cr1 . . 96.77(5) ?
C26 P2 C20 . . 99.66(7) ?
C26 P2 C5 . . 106.62(7) ?
C20 P2 C5 . . 112.64(7) ?
C26 P2 Cr1 . . 124.58(6) ?
C20 P2 Cr1 . . 116.97(5) ?
C5 P2 Cr1 . . 96.31(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.155(2) ?
C1 Cr1 . 1.8484(19) ?
C2 O2 . 1.149(2) ?
C2 Cr1 . 1.8817(17) ?
C3 O3 . 1.151(2) ?
C3 Cr1 . 1.8533(19) ?
C4 O4 . 1.148(2) ?
C4 Cr1 . 1.8860(17) ?
C5 C7 . 1.527(2) ?
C5 C6 . 1.545(2) ?
C5 P1 . 1.8943(16) ?
C5 P2 . 1.8963(17) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C13 . 1.392(3) ?
C8 C9 . 1.393(3) ?
C8 P1 . 1.8393(16) ?
C9 C10 . 1.394(2) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.376(3) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.383(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.394(2) ?
C12 H12 . 0.9500 ?
C13 H13 . 0.9500 ?
C14 C15 . 1.393(3) ?
C14 C19 . 1.399(2) ?
C14 P1 . 1.8184(18) ?
C15 C16 . 1.385(3) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.380(3) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.384(3) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.383(3) ?
C18 H18 . 0.9500 ?
C19 H19 . 0.9500 ?
C20 C25 . 1.391(2) ?
C20 C21 . 1.392(3) ?
C20 P2 . 1.8347(17) ?
C21 C22 . 1.388(3) ?
C21 H21 . 0.9500 ?
C22 C23 . 1.376(3) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.381(3) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.389(3) ?
C24 H24 . 0.9500 ?
C25 H25 . 0.9500 ?
C26 C31 . 1.388(2) ?
C26 C27 . 1.393(3) ?
C26 P2 . 1.8263(16) ?
C27 C28 . 1.384(2) ?
C27 H27 . 0.9500 ?
C28 C29 . 1.380(3) ?
C28 H28 . 0.9500 ?
C29 C30 . 1.373(3) ?
C29 H29 . 0.9500 ?
C30 C31 . 1.391(2) ?
C30 H30 . 0.9500 ?
C31 H31 . 0.9500 ?
C32 Cl2 . 1.737(3) ?
C32 Cl1 . 1.755(3) ?
C32 H32A . 0.9900 ?
C32 H32B . 0.9900 ?
Cr1 P1 . 2.3644(5) ?
Cr1 P2 . 2.3767(5) ?
