#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:10:45 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231527 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/33/4003351.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_4003351
loop_
_publ_author_name
'Zhou, Chenkun'
'Worku, Michael'
'Neu, Jennifer'
'Lin, Haoran'
'Tian, Yu'
'Lee, Sujin'
'Zhou, Yan'
'Han, Dan'
'Chen, Shiyou'
'Hao, Ayou'
'Djurovich, Peter I.'
'Siegrist, Theo'
'Du, Mao-Hua'
'Ma, Biwu'
_publ_section_title
;
 Facile Preparation of Light Emitting Organic Metal Halide Crystals with
 Near-Unity Quantum Efficiency
;
_journal_issue                   7
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2374
_journal_paper_doi               10.1021/acs.chemmater.8b00129
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C48 H40 Cl5 P2 Sb1'
_chemical_formula_sum            'C48 H40 Cl5 P2 Sb'
_chemical_formula_weight         977.81
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                99.3626(18)
_cell_angle_beta                 94.680(2)
_cell_angle_gamma                113.451(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0049(3)
_cell_length_b                   10.0144(2)
_cell_length_c                   12.1801(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1090.12(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54609
_diffrn_reflns_theta_full        32.372
_diffrn_reflns_theta_max         40.978
_diffrn_reflns_theta_min         3.043
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             494
_refine_diff_density_max         2.91
_refine_diff_density_min         -5.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.0004096
_refine_ls_shift/su_mean         0.0000279
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 3.83P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1415
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1415
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7290
_reflns_number_total             13870
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.03
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0684
_oxford_refine_ls_scale          4.01(5)
_oxford_reflns_number_all        8461
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            cm8b00129_si_002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C48 H40 Cl5 P2 Sb1'
_cod_database_code               4003351
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
Sb1 Sb 0.0000 1.0000 1.0000 0.0448 1.0000 Uani S
Cl1 Cl -0.16413(14) 1.08138(14) 0.94780(10) 0.0273 0.5000 Uani .
Cl2 Cl 0.06410(10) 1.00714(9) 0.79675(7) 0.0409 1.0000 Uani .
Cl4 Cl 0.20292(9) 1.27359(8) 1.07156(7) 0.0389 1.0000 Uani .
P9 P 0.38488(7) 0.81503(6) 0.68256(5) 0.0203 1.0000 Uani .
C10 C 0.4825(3) 0.9990(3) 0.76748(19) 0.0234 1.0000 Uani .
C12 C 0.6025(3) 1.1003(3) 0.7313(2) 0.0347 1.0000 Uani .
C13 C 0.6671(4) 1.2491(3) 0.7873(3) 0.0416 1.0000 Uani .
C14 C 0.5117(3) 0.7595(3) 0.6133(2) 0.0236 1.0000 Uani .
C15 C 0.6330(3) 0.7585(3) 0.6782(2) 0.0312 1.0000 Uani .
C16 C 0.2867(3) 0.6806(3) 0.76172(18) 0.0221 1.0000 Uani .
C17 C 0.3314(3) 0.5715(3) 0.7845(2) 0.0277 1.0000 Uani .
C18 C 0.2461(4) 0.4638(3) 0.8394(2) 0.0328 1.0000 Uani .
C19 C 0.1183(3) 0.4666(3) 0.8732(2) 0.0322 1.0000 Uani .
C20 C 0.0749(3) 0.5775(3) 0.8533(2) 0.0292 1.0000 Uani .
C21 C 0.1578(3) 0.6841(3) 0.7963(2) 0.0250 1.0000 Uani .
C22 C 0.2496(2) 0.8158(2) 0.57692(18) 0.0202 1.0000 Uani .
C23 C 0.2422(3) 0.9478(3) 0.5622(2) 0.0238 1.0000 Uani .
C24 C 0.1427(3) 0.9449(3) 0.4742(2) 0.0281 1.0000 Uani .
C25 C 0.0514(3) 0.8116(3) 0.4012(2) 0.0286 1.0000 Uani .
C26 C 0.0563(3) 0.6793(3) 0.4174(2) 0.0269 1.0000 Uani .
C27 C 0.1545(3) 0.6808(3) 0.5053(2) 0.0243 1.0000 Uani .
C2 C 0.4295(3) 1.0460(3) 0.8610(2) 0.0310 1.0000 Uani .
C3 C 0.5865(3) 0.6679(3) 0.4451(3) 0.0332 1.0000 Uani .
C4 C 0.4897(3) 0.7154(3) 0.4958(2) 0.0264 1.0000 Uani .
C5 C 0.4951(4) 1.1950(3) 0.9165(3) 0.0388 1.0000 Uani .
C6 C 0.6131(4) 1.2956(3) 0.8791(3) 0.0386 1.0000 Uani .
C7 C 0.7032(3) 0.6626(3) 0.5102(3) 0.0375 1.0000 Uani .
C8 C 0.7272(3) 0.7081(3) 0.6263(3) 0.0370 1.0000 Uani .
H121 H 0.6401 1.0694 0.6700 0.0411 1.0000 Uiso R
H131 H 0.7494 1.3186 0.7628 0.0489 1.0000 Uiso R
H151 H 0.6515 0.7912 0.7560 0.0359 1.0000 Uiso R
H171 H 0.4192 0.5716 0.7645 0.0321 1.0000 Uiso R
H181 H 0.2740 0.3887 0.8531 0.0377 1.0000 Uiso R
H191 H 0.0620 0.3934 0.9104 0.0380 1.0000 Uiso R
H201 H -0.0087 0.5815 0.8787 0.0339 1.0000 Uiso R
H211 H 0.1265 0.7567 0.7811 0.0288 1.0000 Uiso R
H231 H 0.3037 1.0385 0.6123 0.0268 1.0000 Uiso R
H241 H 0.1376 1.0335 0.4643 0.0333 1.0000 Uiso R
H251 H -0.0149 0.8098 0.3414 0.0333 1.0000 Uiso R
H261 H -0.0039 0.5904 0.3690 0.0309 1.0000 Uiso R
H271 H 0.1573 0.5931 0.5161 0.0286 1.0000 Uiso R
H21 H 0.3505 0.9785 0.8859 0.0360 1.0000 Uiso R
H31 H 0.5720 0.6400 0.3669 0.0393 1.0000 Uiso R
H41 H 0.4095 0.7195 0.4528 0.0300 1.0000 Uiso R
H51 H 0.4589 1.2262 0.9793 0.0450 1.0000 Uiso R
H61 H 0.6568 1.3953 0.9166 0.0462 1.0000 Uiso R
H71 H 0.7665 0.6291 0.4767 0.0442 1.0000 Uiso R
H81 H 0.8084 0.7069 0.6700 0.0431 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sb -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825
4.5909 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl4 2_577 Sb1 Cl2 2_577 89.66(3) yes
Cl4 2_577 Sb1 Cl1 2_577 91.32(4) yes
Cl2 2_577 Sb1 Cl1 2_577 85.45(4) yes
Cl4 2_577 Sb1 Cl1 . 88.68(4) yes
Cl2 2_577 Sb1 Cl1 . 94.55(4) yes
Cl1 2_577 Sb1 Cl1 . 179.995 yes
Cl4 2_577 Sb1 Cl2 . 90.34(3) yes
Cl2 2_577 Sb1 Cl2 . 179.996 yes
Cl1 2_577 Sb1 Cl2 . 94.55(4) yes
Cl1 . Sb1 Cl2 . 85.45(4) yes
Cl4 2_577 Sb1 Cl4 . 179.996 yes
Cl2 2_577 Sb1 Cl4 . 90.34(3) yes
Cl1 2_577 Sb1 Cl4 . 88.68(4) yes
Cl1 . Sb1 Cl4 . 91.32(4) yes
Cl2 . Sb1 Cl4 . 89.66(3) yes
C10 . P9 C14 . 109.41(11) yes
C10 . P9 C16 . 112.97(11) yes
C14 . P9 C16 . 110.23(11) yes
C10 . P9 C22 . 109.06(11) yes
C14 . P9 C22 . 108.39(11) yes
C16 . P9 C22 . 106.64(11) yes
P9 . C10 C12 . 119.07(19) yes
P9 . C10 C2 . 120.68(19) yes
C12 . C10 C2 . 119.8(2) yes
C10 . C12 C13 . 120.0(3) yes
C10 . C12 H121 . 120.4 no
C13 . C12 H121 . 119.6 no
C12 . C13 C6 . 120.0(3) yes
C12 . C13 H131 . 120.2 no
C6 . C13 H131 . 119.8 no
P9 . C14 C15 . 119.20(19) yes
P9 . C14 C4 . 120.97(19) yes
C15 . C14 C4 . 119.8(2) yes
C14 . C15 C8 . 119.8(3) yes
C14 . C15 H151 . 121.0 no
C8 . C15 H151 . 119.3 no
P9 . C16 C17 . 122.07(19) yes
P9 . C16 C21 . 117.76(18) yes
C17 . C16 C21 . 120.1(2) yes
C16 . C17 C18 . 119.9(3) yes
C16 . C17 H171 . 120.2 no
C18 . C17 H171 . 119.9 no
C17 . C18 C19 . 120.0(3) yes
C17 . C18 H181 . 120.3 no
C19 . C18 H181 . 119.7 no
C18 . C19 C20 . 120.4(2) yes
C18 . C19 H191 . 119.1 no
C20 . C19 H191 . 120.5 no
C19 . C20 C21 . 120.1(3) yes
C19 . C20 H201 . 120.2 no
C21 . C20 H201 . 119.7 no
C16 . C21 C20 . 119.5(2) yes
C16 . C21 H211 . 120.7 no
C20 . C21 H211 . 119.8 no
P9 . C22 C23 . 121.48(17) yes
P9 . C22 C27 . 118.54(17) yes
C23 . C22 C27 . 119.9(2) yes
C22 . C23 C24 . 119.7(2) yes
C22 . C23 H231 . 120.0 no
C24 . C23 H231 . 120.3 no
C23 . C24 C25 . 120.3(2) yes
C23 . C24 H241 . 119.8 no
C25 . C24 H241 . 119.9 no
C24 . C25 C26 . 120.0(2) yes
C24 . C25 H251 . 120.3 no
C26 . C25 H251 . 119.6 no
C25 . C26 C27 . 120.1(2) yes
C25 . C26 H261 . 120.4 no
C27 . C26 H261 . 119.5 no
C22 . C27 C26 . 119.9(2) yes
C22 . C27 H271 . 120.1 no
C26 . C27 H271 . 120.1 no
C10 . C2 C5 . 119.7(3) yes
C10 . C2 H21 . 120.0 no
C5 . C2 H21 . 120.3 no
C4 . C3 C7 . 120.1(3) yes
C4 . C3 H31 . 119.2 no
C7 . C3 H31 . 120.6 no
C14 . C4 C3 . 119.6(3) yes
C14 . C4 H41 . 119.1 no
C3 . C4 H41 . 121.3 no
C2 . C5 C6 . 120.2(3) yes
C2 . C5 H51 . 119.4 no
C6 . C5 H51 . 120.4 no
C5 . C6 C13 . 120.3(3) yes
C5 . C6 H61 . 119.9 no
C13 . C6 H61 . 119.8 no
C3 . C7 C8 . 120.6(3) yes
C3 . C7 H71 . 120.3 no
C8 . C7 H71 . 119.1 no
C15 . C8 C7 . 119.9(3) yes
C15 . C8 H81 . 119.8 no
C7 . C8 H81 . 120.3 no
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
Sb1 Cl4 2_577 2.6259(7) yes
Sb1 Cl2 2_577 2.6125(8) yes
Sb1 Cl1 2_577 2.1973(12) yes
Sb1 Cl1 . 2.1973(12) yes
Sb1 Cl2 . 2.6125(8) yes
Sb1 Cl4 . 2.6259(7) yes
P9 C10 . 1.789(2) yes
P9 C14 . 1.794(3) yes
P9 C16 . 1.797(2) yes
P9 C22 . 1.793(2) yes
C10 C12 . 1.388(4) yes
C10 C2 . 1.387(4) yes
C12 C13 . 1.391(4) yes
C12 H121 . 0.927 no
C13 C6 . 1.374(5) yes
C13 H131 . 0.950 no
C14 C15 . 1.398(4) yes
C14 C4 . 1.399(3) yes
C15 C8 . 1.384(4) yes
C15 H151 . 0.927 no
C16 C17 . 1.393(3) yes
C16 C21 . 1.400(4) yes
C17 C18 . 1.392(4) yes
C17 H171 . 0.929 no
C18 C19 . 1.384(4) yes
C18 H181 . 0.934 no
C19 C20 . 1.390(4) yes
C19 H191 . 0.938 no
C20 C21 . 1.393(3) yes
C20 H201 . 0.928 no
C21 H211 . 0.937 no
C22 C23 . 1.392(3) yes
C22 C27 . 1.398(3) yes
C23 C24 . 1.391(4) yes
C23 H231 . 0.943 no
C24 C25 . 1.384(4) yes
C24 H241 . 0.934 no
C25 C26 . 1.391(4) yes
C25 H251 . 0.937 no
C26 C27 . 1.386(3) yes
C26 H261 . 0.921 no
C27 H271 . 0.920 no
C2 C5 . 1.391(4) yes
C2 H21 . 0.924 no
C3 C4 . 1.383(4) yes
C3 C7 . 1.382(5) yes
C3 H31 . 0.929 no
C4 H41 . 0.941 no
C5 C6 . 1.381(5) yes
C5 H51 . 0.933 no
C6 H61 . 0.932 no
C7 C8 . 1.383(5) yes
C7 H71 . 0.919 no
C8 H81 . 0.939 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C4 H41 C27 129 0.94 2.57 3.246(4) yes
