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#$Date: 2018-01-06 03:42:11 +0200 (Sat, 06 Jan 2018) $
#$Revision: 204785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/28/4002873.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_4002873
loop_
_publ_author_name
'Wong, Man Kwong'
'Liu, Fangzhou'
'Kam, Chun Sing'
'Leung, Tik Lun'
'Tam, Ho Won'
'Djurišić, Aleksandra B.'
'Popović, Jasminka'
'Li, Hangkong'
'Shih, Kaimin'
'Low, Kam-Hung'
'Chan, Wai Kin'
'Chen, Wei'
'He, Zhubing'
'Ng, Annie'
'Surya, Charles'
_publ_section_title
;
 Synthesis of Lead-Free Perovskite Films by Combinatorial Evaporation:
 Fast Processes for Screening Different Precursor Combinations
;
_journal_issue                   23
_journal_name_full               'Chemistry of Materials'
_journal_page_first              9946
_journal_paper_doi               10.1021/acs.chemmater.7b03293
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'Br4 Pd, 2(C H6 N)'
_chemical_formula_sum            'C2 H12 Br4 N2 Pd'
_chemical_formula_weight         490.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.604(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9491(4)
_cell_length_b                   10.5856(4)
_cell_length_c                   10.6882(4)
_cell_measurement_reflns_used    274
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     1098.52(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.416
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    16.178
_exptl_absorpt_correction_T_max  0.0401
_exptl_absorpt_correction_T_min  0.0049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.964
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       0.0057(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         2784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0348P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2032
_reflns_number_total             2784
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm7b03293_si_003.cif
_cod_data_source_block           mo_CHEM0422
_cod_depositor_comments
'Adding full bibliography for 4002873--4002875.cif.'
_cod_database_code               4002873
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.104
_shelx_estimated_absorpt_t_max   0.256
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 1.0000 0.5000 0.02006(12) Uani 1 4 d S T P
Pd2 Pd 0.5000 0.5000 0.0000 0.02193(12) Uani 1 4 d S T P
Br1 Br 0.74017(5) 1.0000 0.48541(5) 0.02476(12) Uani 1 2 d S T P
Br2 Br 0.5000 1.22961(5) 0.5000 0.02519(13) Uani 1 2 d S T P
Br3 Br 0.55186(5) 0.5000 -0.21281(5) 0.02837(13) Uani 1 2 d S T P
Br4 Br 0.74801(5) 0.5000 0.09245(6) 0.02783(13) Uani 1 2 d S T P
N1 N 0.6946(4) 0.7425(4) 0.2798(4) 0.0334(8) Uani 1 1 d . . .
H1A H 0.7723 0.7870 0.3134 0.050 Uiso 1 1 calc R U .
H1B H 0.7178 0.6692 0.2452 0.050 Uiso 1 1 calc R U .
H1C H 0.6491 0.7244 0.3428 0.050 Uiso 1 1 calc R U .
C1 C 0.6044(5) 0.8185(5) 0.1786(5) 0.0401(10) Uani 1 1 d . . .
H3 H 0.5763 0.8958 0.2165 0.060 Uiso 1 1 calc R U .
H1 H 0.5225 0.7692 0.1400 0.060 Uiso 1 1 calc R U .
H2 H 0.6547 0.8408 0.1125 0.060 Uiso 1 1 calc R U .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
Br1 Pd1 Br1 180.0 5_676 .
Br1 Pd1 Br2 90.0 5_676 5_676
Br1 Pd1 Br2 90.0 . 5_676
Br1 Pd1 Br2 90.0 5_676 .
Br1 Pd1 Br2 90.0 . .
Br2 Pd1 Br2 180.0 5_676 .
Br3 Pd2 Br3 180.0 5_665 .
Br3 Pd2 Br4 91.332(19) 5_665 .
Br3 Pd2 Br4 88.668(19) . .
Br3 Pd2 Br4 88.668(19) 5_665 5_665
Br3 Pd2 Br4 91.332(19) . 5_665
Br4 Pd2 Br4 180.0 . 5_665
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N1 C1 H3 109.5 . .
N1 C1 H1 109.5 . .
H3 C1 H1 109.5 . .
N1 C1 H2 109.5 . .
H3 C1 H2 109.5 . .
H1 C1 H2 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Br1 2.4282(5) 5_676
Pd1 Br1 2.4283(5) .
Pd1 Br2 2.4305(5) 5_676
Pd1 Br2 2.4306(5) .
Pd2 Br3 2.4396(6) 5_665
Pd2 Br3 2.4396(6) .
Pd2 Br4 2.4497(5) .
Pd2 Br4 2.4497(5) 5_665
N1 C1 1.483(6) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
C1 H3 0.9800 .
C1 H1 0.9800 .
C1 H2 0.9800 .
