#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/41/2204121.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2204121
loop_
_publ_author_name
'Light, Mark E.'
'Hursthouse, Michael B.'
'Beckett, Michael A.'
'Brassington, David S.'
_publ_section_title
;
 A mixed-halogen tricarbonylmanganese(I) complex:
 fac-[MnBr~0.3~Cl~0.7~{Ph₂P(CH₂)₃PPh₂}(CO)₃]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1245
_journal_page_last               m1247
_journal_paper_doi               10.1107/S1600536804019385
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Mn Br0.3 Cl0.7 (C30 H26 O3 P2) (C O)3]'
_chemical_formula_moiety         'C30 H26 Br0.30 Cl0.70 Mn O3 P2'
_chemical_formula_sum            'C30 H26 Br0.3 Cl0.7 Mn O3 P2'
_chemical_formula_weight         600.18
_chemical_name_systematic
;
fac-(bromo/chloro)tricarbonyl[1,3-bis(diphenylphosphino)propane]manganese(I)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.0900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.00220(10)
_cell_length_b                   20.6821(3)
_cell_length_c                   13.7320(2)
_cell_measurement_reflns_used    26531
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2729.41(6)
_computing_cell_refinement
;
DENZO and COLLECT
;
_computing_data_collection
;
DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_data_reduction
;
DENZO and COLLECT
;
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WinGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9102
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8042
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0274P)²+2.0712P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                4504
_reflns_number_total             4792
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br6160.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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/n'
_cod_original_formula_sum        'C30 H26 Br0.30 Cl0.70 Mn O3 P2'
_cod_database_code               2204121
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_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_type_symbol
Mn1 0.03367(2) 0.111790(12) 0.265369(18) 0.01346(8) Uani d . 1 Mn
Br1 -0.1243(11) 0.0727(6) 0.3637(10) 0.0162(7) Uani d P 0.30 Br
Cl1 -0.1078(11) 0.0692(7) 0.3641(10) 0.0162(7) Uani d P 0.70 Cl
O1 -0.17174(14) 0.07553(7) 0.07242(10) 0.0291(3) Uani d . 1 O
O2 -0.11973(16) 0.23550(7) 0.25914(11) 0.0379(4) Uani d . 1 O
O3 0.20117(14) 0.17777(6) 0.15057(10) 0.0270(3) Uani d . 1 O
P1 0.13301(4) 0.00811(2) 0.26973(3) 0.01222(10) Uani d . 1 P
P2 0.18760(4) 0.13453(2) 0.42487(3) 0.01407(10) Uani d . 1 P
C1 -0.09344(18) 0.08870(8) 0.14755(13) 0.0184(4) Uani d . 1 C
C2 -0.05856(19) 0.18841(9) 0.26435(14) 0.0225(4) Uani d . 1 C
C3 0.13873(18) 0.15005(8) 0.19651(13) 0.0179(4) Uani d . 1 C
C4 0.02199(17) -0.05725(8) 0.20019(12) 0.0152(3) Uani d . 1 C
C5 -0.11268(18) -0.06423(9) 0.20913(14) 0.0209(4) Uani d . 1 C
H5 -0.1482 -0.0335 0.2470 0.025 Uiso calc R 1 H
C6 -0.19555(19) -0.11584(9) 0.16293(15) 0.0243(4) Uani d . 1 C
H6 -0.2868 -0.1205 0.1702 0.029 Uiso calc R 1 H
C7 -0.1459(2) -0.16034(9) 0.10662(15) 0.0267(4) Uani d . 1 C
H7 -0.2030 -0.1952 0.0745 0.032 Uiso calc R 1 H
C8 -0.0129(2) -0.15383(10) 0.09721(16) 0.0310(5) Uani d . 1 C
H8 0.0216 -0.1846 0.0588 0.037 Uiso calc R 1 H
C9 0.0714(2) -0.10268(9) 0.14347(15) 0.0249(4) Uani d . 1 C
H9 0.1628 -0.0987 0.1364 0.030 Uiso calc R 1 H
C10 0.28325(17) 0.00516(8) 0.21874(12) 0.0142(3) Uani d . 1 C
C11 0.26862(18) 0.03101(8) 0.12253(13) 0.0174(4) Uani d . 1 C
H11 0.1800 0.0457 0.0834 0.021 Uiso calc R 1 H
C12 0.38202(19) 0.03546(9) 0.08333(13) 0.0211(4) Uani d . 1 C
H12 0.3705 0.0528 0.0174 0.025 Uiso calc R 1 H
C13 0.51196(19) 0.01480(9) 0.13984(14) 0.0242(4) Uani d . 1 C
H13 0.5902 0.0193 0.1140 0.029 Uiso calc R 1 H
C14 0.52714(19) -0.01247(10) 0.23413(14) 0.0244(4) Uani d . 1 C
H14 0.6158 -0.0275 0.2725 0.029 Uiso calc R 1 H
C15 0.41331(18) -0.01803(9) 0.27334(13) 0.0195(4) Uani d . 1 C
H15 0.4243 -0.0377 0.3376 0.023 Uiso calc R 1 H
C16 0.19140(17) -0.03009(8) 0.39487(12) 0.0143(3) Uani d . 1 C
H16A 0.1078 -0.0419 0.4162 0.017 Uiso calc R 1 H
H16B 0.2396 -0.0708 0.3875 0.017 Uiso calc R 1 H
C17 0.28795(17) 0.00913(8) 0.48050(12) 0.0154(3) Uani d . 1 C
H17A 0.3254 -0.0197 0.5393 0.019 Uiso calc R 1 H
H17B 0.3675 0.0251 0.4576 0.019 Uiso calc R 1 H
C18 0.21637(18) 0.06682(8) 0.51456(12) 0.0162(4) Uani d . 1 C
H18A 0.2742 0.0818 0.5814 0.019 Uiso calc R 1 H
H18B 0.1256 0.0526 0.5229 0.019 Uiso calc R 1 H
C19 0.36961(17) 0.15668(8) 0.43925(13) 0.0177(4) Uani d . 1 C
C20 0.43408(18) 0.14319(9) 0.36369(15) 0.0218(4) Uani d . 1 C
H20 0.3802 0.1276 0.2998 0.026 Uiso calc R 1 H
C21 0.57690(19) 0.15236(9) 0.38088(17) 0.0284(4) Uani d . 1 C
H21 0.6198 0.1436 0.3286 0.034 Uiso calc R 1 H
C22 0.6558(2) 0.17423(9) 0.47422(17) 0.0311(5) Uani d . 1 C
H22 0.7533 0.1800 0.4863 0.037 Uiso calc R 1 H
C23 0.5935(2) 0.18763(9) 0.54982(17) 0.0305(5) Uani d . 1 C
H23 0.6484 0.2025 0.6139 0.037 Uiso calc R 1 H
C24 0.4510(2) 0.17953(9) 0.53306(15) 0.0248(4) Uani d . 1 C
H24 0.4087 0.1895 0.5852 0.030 Uiso calc R 1 H
C25 0.12680(18) 0.19939(8) 0.49242(13) 0.0187(4) Uani d . 1 C
C26 0.1334(2) 0.26315(9) 0.46047(15) 0.0255(4) Uani d . 1 C
H26 0.1734 0.2724 0.4068 0.031 Uiso calc R 1 H
C27 0.0813(2) 0.31328(10) 0.50727(17) 0.0325(5) Uani d . 1 C
H27 0.0854 0.3566 0.4850 0.039 Uiso calc R 1 H
C28 0.0240(2) 0.30034(10) 0.58568(16) 0.0341(5) Uani d . 1 C
H28 -0.0110 0.3347 0.6174 0.041 Uiso calc R 1 H
C29 0.0174(2) 0.23756(11) 0.61824(16) 0.0322(5) Uani d . 1 C
H29 -0.0219 0.2288 0.6724 0.039 Uiso calc R 1 H
C30 0.06850(19) 0.18705(9) 0.57143(14) 0.0238(4) Uani d . 1 C
H30 0.0634 0.1439 0.5937 0.029 Uiso calc R 1 H
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C3 Mn1 C1 90.81(8) n
C3 Mn1 C2 88.95(8) n
C1 Mn1 C2 89.65(8) n
C3 Mn1 P2 94.32(6) n
C1 Mn1 P2 174.68(6) n
C2 Mn1 P2 91.86(6) n
C3 Mn1 P1 96.37(6) n
C1 Mn1 P1 88.26(5) n
C2 Mn1 P1 174.31(6) n
P2 Mn1 P1 89.754(16) n
C3 Mn1 Cl1 175.2(3) n
C1 Mn1 Cl1 91.7(3) n
C2 Mn1 Cl1 87.0(3) n
P2 Mn1 Cl1 83.3(3) n
P1 Mn1 Cl1 87.8(3) n
C3 Mn1 Br1 172.6(3) n
C1 Mn1 Br1 90.3(3) n
C2 Mn1 Br1 83.7(3) n
P2 Mn1 Br1 84.8(3) n
P1 Mn1 Br1 91.0(3) n
Cl1 Mn1 Br1 3.5(5) n
C10 P1 C16 105.23(8) n
C10 P1 C4 102.65(8) n
C16 P1 C4 99.18(7) n
C10 P1 Mn1 113.99(5) n
C16 P1 Mn1 115.99(5) n
C4 P1 Mn1 117.75(5) n
C25 P2 C19 102.82(8) n
C25 P2 C18 103.41(8) n
C19 P2 C18 98.75(8) n
C25 P2 Mn1 113.31(6) n
C19 P2 Mn1 121.66(6) n
C18 P2 Mn1 114.42(6) n
O1 C1 Mn1 178.16(16) n
O2 C2 Mn1 176.75(17) n
O3 C3 Mn1 175.96(15) n
C5 C4 C9 118.68(16) n
C5 C4 P1 119.31(13) n
C9 C4 P1 121.89(13) n
C6 C5 C4 120.49(17) n
C6 C5 H5 119.8 n
C4 C5 H5 119.8 n
C7 C6 C5 120.35(18) n
C7 C6 H6 119.8 n
C5 C6 H6 119.8 n
C8 C7 C6 119.62(17) n
C8 C7 H7 120.2 n
C6 C7 H7 120.2 n
C7 C8 C9 120.65(18) n
C7 C8 H8 119.7 n
C9 C8 H8 119.7 n
C8 C9 C4 120.22(17) n
C8 C9 H9 119.9 n
C4 C9 H9 119.9 n
C15 C10 C11 118.59(15) n
C15 C10 P1 123.33(13) n
C11 C10 P1 117.96(13) n
C12 C11 C10 120.71(16) n
C12 C11 H11 119.6 n
C10 C11 H11 119.6 n
C13 C12 C11 120.26(16) n
C13 C12 H12 119.9 n
C11 C12 H12 119.9 n
C14 C13 C12 119.60(17) n
C14 C13 H13 120.2 n
C12 C13 H13 120.2 n
C13 C14 C15 120.45(17) n
C13 C14 H14 119.8 n
C15 C14 H14 119.8 n
C14 C15 C10 120.31(16) n
C14 C15 H15 119.8 n
C10 C15 H15 119.8 n
C17 C16 P1 117.45(11) n
C17 C16 H16A 107.9 n
P1 C16 H16A 107.9 n
C17 C16 H16B 107.9 n
P1 C16 H16B 107.9 n
H16A C16 H16B 107.2 n
C18 C17 C16 113.51(14) n
C18 C17 H17A 108.9 n
C16 C17 H17A 108.9 n
C18 C17 H17B 108.9 n
C16 C17 H17B 108.9 n
H17A C17 H17B 107.7 n
C17 C18 P2 112.94(12) n
C17 C18 H18A 109.0 n
P2 C18 H18A 109.0 n
C17 C18 H18B 109.0 n
P2 C18 H18B 109.0 n
H18A C18 H18B 107.8 n
C20 C19 C24 118.76(16) n
C20 C19 P2 121.35(13) n
C24 C19 P2 119.31(14) n
C19 C20 C21 120.69(18) n
C19 C20 H20 119.7 n
C21 C20 H20 119.7 n
C22 C21 C20 119.8(2) n
C22 C21 H21 120.1 n
C20 C21 H21 120.1 n
C23 C22 C21 120.18(18) n
C23 C22 H22 119.9 n
C21 C22 H22 119.9 n
C22 C23 C24 120.54(19) n
C22 C23 H23 119.7 n
C24 C23 H23 119.7 n
C23 C24 C19 120.05(19) n
C23 C24 H24 120.0 n
C19 C24 H24 120.0 n
C30 C25 C26 119.00(17) n
C30 C25 P2 122.12(14) n
C26 C25 P2 118.81(14) n
C27 C26 C25 120.06(19) n
C27 C26 H26 120.0 n
C25 C26 H26 120.0 n
C28 C27 C26 120.31(19) n
C28 C27 H27 119.8 n
C26 C27 H27 119.8 n
C27 C28 C29 120.20(18) n
C27 C28 H28 119.9 n
C29 C28 H28 119.9 n
C28 C29 C30 119.9(2) n
C28 C29 H29 120.1 n
C30 C29 H29 120.1 n
C25 C30 C29 120.56(19) n
C25 C30 H30 119.7 n
C29 C30 H30 119.7 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 C3 1.7820(19) y
Mn1 C1 1.8226(18) y
Mn1 C2 1.8317(19) y
Mn1 P2 2.3495(5) y
Mn1 P1 2.3572(5) y
Mn1 Cl1 2.384(13) y
Mn1 Br1 2.481(13) y
O1 C1 1.142(2) n
O2 C2 1.142(2) n
O3 C3 1.155(2) n
P1 C10 1.8263(17) n
P1 C16 1.8335(16) n
P1 C4 1.8397(17) n
P2 C25 1.8281(18) n
P2 C19 1.8340(17) n
P2 C18 1.8343(17) n
C4 C5 1.393(2) n
C4 C9 1.395(3) n
C5 C6 1.392(3) n
C5 H5 0.9500 n
C6 C7 1.380(3) n
C6 H6 0.9500 n
C7 C8 1.378(3) n
C7 H7 0.9500 n
C8 C9 1.392(3) n
C8 H8 0.9500 n
C9 H9 0.9500 n
C10 C15 1.394(2) n
C10 C11 1.395(2) n
C11 C12 1.387(3) n
C11 H11 0.9500 n
C12 C13 1.384(3) n
C12 H12 0.9500 n
C13 C14 1.382(3) n
C13 H13 0.9500 n
C14 C15 1.393(3) n
C14 H14 0.9500 n
C15 H15 0.9500 n
C16 C17 1.531(2) n
C16 H16A 0.9900 n
C16 H16B 0.9900 n
C17 C18 1.530(2) n
C17 H17A 0.9900 n
C17 H17B 0.9900 n
C18 H18A 0.9900 n
C18 H18B 0.9900 n
C19 C20 1.393(3) n
C19 C24 1.402(3) n
C20 C21 1.395(3) n
C20 H20 0.9500 n
C21 C22 1.382(3) n
C21 H21 0.9500 n
C22 C23 1.379(3) n
C22 H22 0.9500 n
C23 C24 1.389(3) n
C23 H23 0.9500 n
C24 H24 0.9500 n
C25 C30 1.390(3) n
C25 C26 1.397(3) n
C26 C27 1.395(3) n
C26 H26 0.9500 n
C27 C28 1.379(3) n
C27 H27 0.9500 n
C28 C29 1.381(3) n
C28 H28 0.9500 n
C29 C30 1.396(3) n
C29 H29 0.9500 n
C30 H30 0.9500 n
